Пожалуйста, помогите найти две статьи из Annali di Chimica:
1) Ridi, Checchi. 1953. 43. 816-822.
2) De Martiis, Toffoli. 1957. 47. 1232-1237.
Заранее благодарен.
+++Annali di Chimica
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alchemist1305
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+++Annali di Chimica
Последний раз редактировалось alchemist1305 Чт июл 09, 2009 6:02 pm, всего редактировалось 1 раз.
Re: Annali di Chimica
ГПНТБ и то надо год смотреть!
Заказал ждем-с
Заказал ждем-с
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
Re: Annali di Chimica
Ждите скан
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
Re: Annali di Chimica
Вот проверяем плюсики не забываем
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
-
alchemist1305
- Сообщения: 79
- Зарегистрирован: Вт июн 16, 2009 2:49 pm
Re: Annali di Chimica
Только вот статья, обозначенная как Annali di chimica 1953, увы не та (((. А за вторую спасибо!
Re: Annali di Chimica
Да действиетльно не та старнно! надо перезаказывать!
Как я могу не тот год заказать не знаю! Хотя подозреваю!
До сих пор удивляюсь как можно было заказть нетот год или тот не принесли а этот остался уменя не знаю вот это уточним еще раз
New derivatives of antipyrine, isoantipyrine, and pyrazolidine. Ridi, Mario; Checchi, Silvio. Univ. Florence, Annali di Chimica (Rome, Italy) (1953), 43 816-26. CA 49:32372
Abstract
A no. of compds. has been synthesized as potential pharmaceuticals. Equimol. amts. of antipyraldehyde (I, R = OHC) (II) and o-C6H4(NH2)2 dissolved in alc., cooled 1 hr. on ice, and scratched with a glass rod gave the corresponding Schiff base (I, R = o-H2NC6H4N:CH) (III), m. 215° (purified by washing with alc. and water); a dioxane soln. boiled 5 hrs. and evapd. to a small vol. deposited 4-(2-benzimidazolyl)-antipyrine (IV), m. 280° (recrystd. from dioxane and washed with hot AcOEt). III gave IV also when heated 1 hr. at 200°, taken up in 1:1 alc.-dioxane, decolorized, and cooled. III (0.2 g.) in AcOH boiled 10 min. with 0.3 g. PhNHNH2 produced on cooling and addn. of water the phenylhydrazone (I, R = PhNHN:CH) of II, m. 254°, also obtained by sapon. of III with KOH, acidification with AcOH, and addn. of PhNHNH2. Under similar conditions IV did not react with PhNHNH2.AcOH. "Isoantipyrine" (V, R = H) heated with an equal wt. of CCl3CHO.H2O 5 hrs. at 130°, the product dissolved in alc., and water added gave a crystallizable oil, which, recrystd. from 90% alc. and 1:1 alc.-dioxane with C, gave V[R = CCl3CH(OH)] (VI), m. 190-3°. VI (4.2 g.) boiled 15 min. in 7.5 cc. cold satd. K2CO3 soln. evolved CHCl3 and formed an oil solidifying on cooling to a yellow-brown solid which was washed with water, dried, and extd. several times with ether; from the ether ext. was isolated V (R = OHC) (VII), m. 138° (from AcOEt), and from the residue an unidentified compd., m. 285°. VII (0.26 g.) in alc. with 0.105 g. PhNHNH2 gave a phenylhydrazone, m. 230-5° (from AcOH); an oxime (from 1.08 g. VII, 0.78 g. NH2OH.HCl, and 1 g. NaOAc boiled briefly in a little water), m. 221-2°; and a thiosemicarbazone (from 0.432 g. VII and 0.102 g. H2NCSNHNH2 in 2 cc. 60% alc. boiled 30 min.), m. 238° (decompn.) (from alc.). Heating 0.216 g. VII 1 hr. at 100° with 0.137 g. p-phenetidine and 1 g. K2CO3 gave V (R = p-EtOC4H4N:CH), m. 135° (from AcOEt). Equimol. amts. of malonylurea and VII in alc. boiled until complete pptn.
of V (R = CO.NH.CO.NH.CO.C:CH), m. 268°. Similarly, 3-phenylbarbituric acid gave V (R = CO.NPh.CO.NH.CO.C:CH), m. 276°. VII (1.08 g.) in 10 cc. anhyd. MeOH treated with 0.44 g. recently distd. AcCO2H, then gradually with 0.72 g. 2-C10H7NH2 in 10 cc. anhyd. MeOH, the mixt. refluxed 4 hrs., and the ppt. dissolved in alkali, repptd. with HCl, and washed with hot alc. produced 2-(2-phenyl-1,3-dimethyl-5-oxo-3-pyrazolin-4-yl)-6,7-benzocinchoninic acid, m. 278° (decompn.). CCl3CHO.H2O (1 g.) added to 1 g. IX (R = H) and the mixt. kept 2 hrs. at 120° and taken up in 1:1 aq. alc. deposited IX [R = CCl3CH(OH)], m. 182-5° (from AcOEt), 4.2 g. of which, suspended in 7.5 cc. cold satd. K2CO3 soln. and boiled, gave off CHCl3 and formed a crystallizable oil IX (R = OHC) (X), m. 155° (from EtOAc). X and VII, heated 15 min. at 150° with an equiv. amt. of XI (R = H), lose their CHO group; the dark tarry product, taken up in alc., yields a yellow-orange compd. (XI, R = CO.NPh.N:CMe.C:CH), m. 181°, and, from the mother liquors, the unsubstituted pyrazolinones IX and V (R = H). XII (R = PhN:CH) (XIII), m. 268°, was prepd. from equimol. amts. of XII (R = H) and HC(:NPh)-NHPh heated 40 min. at 130° and purified from AcOH. XII (R = p-EtOC6H4N:CH) (XIV), m. 270°, was obtained like XIII from HC(:NR')NHR' (R' = p-EtOC6H4) and recrystd. from dioxane. XII (R = OHC) (XV), m. 233-5°, was formed by suspending 1 g. XIII or XIV in 15 cc. 10% KOH, extg. the PhNH2 or p-phenetidine formed with ether, evapg. the soln. to a small vol., cooling, acidifying with HCl, and crystg. the oil, which soon solidified, from AcOH-AcOEt. XV formed a phenylhydrazone, m. 190°, by boiling with PhNHNH2 in AcOH. Equimol. amts. of XV and barbituric acid kept 30 min. in AcOH gave XII (R = CO.NH.CO.NH.CO.C:CH) (XVI), m. 296°. Equimol. amts. of XV and XIII boiled 1 hr. in AcOH gave XII (R = CO.NH.NPh.CO.C:CH) (XVII), m. 310° (decompn.). Similarly XV and XI (R = H) gave XII (R = CMe:N.NPh.CO.C:CH (XVIII), m. 262°; fusion of the 2 compds. 10 min.
at 160° gave XI. 1-Methyl-3-phenyl-3-pyrazolin-5-one gave the 4-CCl3CH(OH) deriv., m. 184°, when heated with an equimol. amt. of CCl3CHO.H2O 3 hrs. at 120°, and the 4-NC deriv., m. 225°, from 1.7 g. of the pyrazolinone in 20 cc. alc. added to 4 g. Hg fulminate and 2 g. KI in 15 cc. water, heated 15 min. at 50°, boiled 1 hr., satd. with H2S, decolorized, the soln. concd., and the ppt. crystd. from AcOEt. Other aldimines, o-H2NC6H4N:CHCH.CO.NR'.N:CR, analogous to III were prepd. from o-C6H4(NH2)2 and 4-formyl-3-pyrazolin-5-ones by keeping equimol. amts. 1 hr. in cold C6H6 (R and R' given): Me, p-EtOC6H4, m. 195°; Ph, Ph, m. 215°; Me, Ph, no m.p. given. Another mol. of the aldehyde with the di-Ph compd. gave the dialdimine, C38H28O2N6, m. 225°, and the R = Me, R = Ph compd. gave the corresponding dialdimine, m. 260° (from dioxane), which yielded XI after 3 hrs. boiling in PhNO2. Equimol. amts. of 1-phenyl-5-(aminomethylene)barbituric acid [or the 5-(hydroxymethylene) analog] in hot alc. [or in cold dioxane] yielded o-H2NC6H4N:CHCH.CO.NPh.CO.NH.CO, m. 250°. Similarly, o-C6H4(NH2)2 and 1,3-diphenyl-5-(aminomethylene)-2-thiobarbituric acid gave o-H2NC6H4N:CHCH.CO.NPh.CS.NPh.CO, m. 255°.
По моему в абстракте больше чем в самой тсатье
))
Будем перезаказывать, единственно могло не прийти еще и я по шибке сдела ксерокс другой! НО мало вероятно вторая то пришла нормлаьно! Ну ладно че гадать перезакажу!
Как я могу не тот год заказать не знаю! Хотя подозреваю!
До сих пор удивляюсь как можно было заказть нетот год или тот не принесли а этот остался уменя не знаю вот это уточним еще раз
New derivatives of antipyrine, isoantipyrine, and pyrazolidine. Ridi, Mario; Checchi, Silvio. Univ. Florence, Annali di Chimica (Rome, Italy) (1953), 43 816-26. CA 49:32372
Abstract
A no. of compds. has been synthesized as potential pharmaceuticals. Equimol. amts. of antipyraldehyde (I, R = OHC) (II) and o-C6H4(NH2)2 dissolved in alc., cooled 1 hr. on ice, and scratched with a glass rod gave the corresponding Schiff base (I, R = o-H2NC6H4N:CH) (III), m. 215° (purified by washing with alc. and water); a dioxane soln. boiled 5 hrs. and evapd. to a small vol. deposited 4-(2-benzimidazolyl)-antipyrine (IV), m. 280° (recrystd. from dioxane and washed with hot AcOEt). III gave IV also when heated 1 hr. at 200°, taken up in 1:1 alc.-dioxane, decolorized, and cooled. III (0.2 g.) in AcOH boiled 10 min. with 0.3 g. PhNHNH2 produced on cooling and addn. of water the phenylhydrazone (I, R = PhNHN:CH) of II, m. 254°, also obtained by sapon. of III with KOH, acidification with AcOH, and addn. of PhNHNH2. Under similar conditions IV did not react with PhNHNH2.AcOH. "Isoantipyrine" (V, R = H) heated with an equal wt. of CCl3CHO.H2O 5 hrs. at 130°, the product dissolved in alc., and water added gave a crystallizable oil, which, recrystd. from 90% alc. and 1:1 alc.-dioxane with C, gave V[R = CCl3CH(OH)] (VI), m. 190-3°. VI (4.2 g.) boiled 15 min. in 7.5 cc. cold satd. K2CO3 soln. evolved CHCl3 and formed an oil solidifying on cooling to a yellow-brown solid which was washed with water, dried, and extd. several times with ether; from the ether ext. was isolated V (R = OHC) (VII), m. 138° (from AcOEt), and from the residue an unidentified compd., m. 285°. VII (0.26 g.) in alc. with 0.105 g. PhNHNH2 gave a phenylhydrazone, m. 230-5° (from AcOH); an oxime (from 1.08 g. VII, 0.78 g. NH2OH.HCl, and 1 g. NaOAc boiled briefly in a little water), m. 221-2°; and a thiosemicarbazone (from 0.432 g. VII and 0.102 g. H2NCSNHNH2 in 2 cc. 60% alc. boiled 30 min.), m. 238° (decompn.) (from alc.). Heating 0.216 g. VII 1 hr. at 100° with 0.137 g. p-phenetidine and 1 g. K2CO3 gave V (R = p-EtOC4H4N:CH), m. 135° (from AcOEt). Equimol. amts. of malonylurea and VII in alc. boiled until complete pptn.
of V (R = CO.NH.CO.NH.CO.C:CH), m. 268°. Similarly, 3-phenylbarbituric acid gave V (R = CO.NPh.CO.NH.CO.C:CH), m. 276°. VII (1.08 g.) in 10 cc. anhyd. MeOH treated with 0.44 g. recently distd. AcCO2H, then gradually with 0.72 g. 2-C10H7NH2 in 10 cc. anhyd. MeOH, the mixt. refluxed 4 hrs., and the ppt. dissolved in alkali, repptd. with HCl, and washed with hot alc. produced 2-(2-phenyl-1,3-dimethyl-5-oxo-3-pyrazolin-4-yl)-6,7-benzocinchoninic acid, m. 278° (decompn.). CCl3CHO.H2O (1 g.) added to 1 g. IX (R = H) and the mixt. kept 2 hrs. at 120° and taken up in 1:1 aq. alc. deposited IX [R = CCl3CH(OH)], m. 182-5° (from AcOEt), 4.2 g. of which, suspended in 7.5 cc. cold satd. K2CO3 soln. and boiled, gave off CHCl3 and formed a crystallizable oil IX (R = OHC) (X), m. 155° (from EtOAc). X and VII, heated 15 min. at 150° with an equiv. amt. of XI (R = H), lose their CHO group; the dark tarry product, taken up in alc., yields a yellow-orange compd. (XI, R = CO.NPh.N:CMe.C:CH), m. 181°, and, from the mother liquors, the unsubstituted pyrazolinones IX and V (R = H). XII (R = PhN:CH) (XIII), m. 268°, was prepd. from equimol. amts. of XII (R = H) and HC(:NPh)-NHPh heated 40 min. at 130° and purified from AcOH. XII (R = p-EtOC6H4N:CH) (XIV), m. 270°, was obtained like XIII from HC(:NR')NHR' (R' = p-EtOC6H4) and recrystd. from dioxane. XII (R = OHC) (XV), m. 233-5°, was formed by suspending 1 g. XIII or XIV in 15 cc. 10% KOH, extg. the PhNH2 or p-phenetidine formed with ether, evapg. the soln. to a small vol., cooling, acidifying with HCl, and crystg. the oil, which soon solidified, from AcOH-AcOEt. XV formed a phenylhydrazone, m. 190°, by boiling with PhNHNH2 in AcOH. Equimol. amts. of XV and barbituric acid kept 30 min. in AcOH gave XII (R = CO.NH.CO.NH.CO.C:CH) (XVI), m. 296°. Equimol. amts. of XV and XIII boiled 1 hr. in AcOH gave XII (R = CO.NH.NPh.CO.C:CH) (XVII), m. 310° (decompn.). Similarly XV and XI (R = H) gave XII (R = CMe:N.NPh.CO.C:CH (XVIII), m. 262°; fusion of the 2 compds. 10 min.
at 160° gave XI. 1-Methyl-3-phenyl-3-pyrazolin-5-one gave the 4-CCl3CH(OH) deriv., m. 184°, when heated with an equimol. amt. of CCl3CHO.H2O 3 hrs. at 120°, and the 4-NC deriv., m. 225°, from 1.7 g. of the pyrazolinone in 20 cc. alc. added to 4 g. Hg fulminate and 2 g. KI in 15 cc. water, heated 15 min. at 50°, boiled 1 hr., satd. with H2S, decolorized, the soln. concd., and the ppt. crystd. from AcOEt. Other aldimines, o-H2NC6H4N:CHCH.CO.NR'.N:CR, analogous to III were prepd. from o-C6H4(NH2)2 and 4-formyl-3-pyrazolin-5-ones by keeping equimol. amts. 1 hr. in cold C6H6 (R and R' given): Me, p-EtOC6H4, m. 195°; Ph, Ph, m. 215°; Me, Ph, no m.p. given. Another mol. of the aldehyde with the di-Ph compd. gave the dialdimine, C38H28O2N6, m. 225°, and the R = Me, R = Ph compd. gave the corresponding dialdimine, m. 260° (from dioxane), which yielded XI after 3 hrs. boiling in PhNO2. Equimol. amts. of 1-phenyl-5-(aminomethylene)barbituric acid [or the 5-(hydroxymethylene) analog] in hot alc. [or in cold dioxane] yielded o-H2NC6H4N:CHCH.CO.NPh.CO.NH.CO, m. 250°. Similarly, o-C6H4(NH2)2 and 1,3-diphenyl-5-(aminomethylene)-2-thiobarbituric acid gave o-H2NC6H4N:CHCH.CO.NPh.CS.NPh.CO, m. 255°.
По моему в абстракте больше чем в самой тсатье
))Будем перезаказывать, единственно могло не прийти еще и я по шибке сдела ксерокс другой! НО мало вероятно вторая то пришла нормлаьно! Ну ладно че гадать перезакажу!
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
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alchemist1305
- Сообщения: 79
- Зарегистрирован: Вт июн 16, 2009 2:49 pm
Re: Annali di Chimica
Ну что Вы еще не пробовали перезаказать? 
Re: Annali di Chimica
Перезаказал жлдем-с!
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
Re: Annali di Chimica
Первой ждите скан я достал ее вроде она и год вроде тот!
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
Re: Annali di Chimica
Вот проверяем плюсики не забываем!
"Ничто так не воодушевляет, как осознание своего безнадежного положения." Альбер Камю.
-
alchemist1305
- Сообщения: 79
- Зарегистрирован: Вт июн 16, 2009 2:49 pm
Re: Annali di Chimica
ОГРОМНОЕ СПАСИБО!!!
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