+++Поиск по Reaxys_Спасибо

[paramona]

Коллеги, пожалуйста, помогите найти методики синтеза по приведенным структурам (получение и физ. хим. свойства), и если эти соединения описаны, то где конкретно.

1) CC(=O)c1nc(N)sc1C

2) Cc1sc(N)nc1C(=O)CBr

Заранее благодарен.

[mishka]

есть свойства и получение только 2-Amino-4-acetyl-5-methylthiazol

свойства

Melting Point, °C Reference
140 - 141
Sarkis; Al-Azawe[Journal of Chemical and Engineering Data, 1973, vol. 18, p. 99,100]


Colour & Other Properties Location Reference
white
Paragraph 0353
Current Patent Assignee: GENENTECH - WO2015/52226, 2015, A1

Description (Further Information) Reference
Further information
Alazawe; Bakir[Bulletin of the College of Science, University of Baghdad, 1972, vol. 12-13, p.
91,94]


ЯМР, УФ и ИК в
Sarkis; Al-Azawe[Journal of Chemical and Engineering Data, 1973, vol. 18, p. 99,100]


Description (Mass Spectrometry) Location Reference
liquid chromatography mass spectrometry (LCMS), electrospray ionisation (ESI), spectrum
Paragraph 0351
Current Patent Assignee: GENENTECH - WO2015/52226, 2015, A1

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получение
Тиомочевина + 4-bromopentane-2,3-dione = 2-Amino-4-acetyl-5-methylthiazol

In ethanol for 3h; Hantzsch thiazole synthesis; Reflux;
Walter; Von Coburg; Isensee; Sander; Ligneau; Camelin; Schwartz; Stark
[Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 19, p. 5879 - 5882]


In ethanol at 100℃; for 1h;
1.2 g
Current Patent Assignee: GENENTECH - WO2015/52226, 2015, A1
Location in patent: Paragraph 0353


In ethanol Reflux;
Volgraf, Matthew; Sellers, Benjamin D.; Jiang, Yu; Wu, Guosheng; Ly, Cuong Q.; Villemure, Elisia;

Pastor, Richard M.; (…) Scearce-Levie, Kimberly; Schwarz, Jacob B.
[Journal of Medicinal Chemistry, 2016, vol. 59, # 6, p. 2760 - 2779]

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из 2,3-Pentanedione

Multi-step reaction with 2 steps
1: hydrogen bromide; acetic acid; bromine / chloroform / 3 h / 50 °C
2: ethanol / 1 h / 100 °C

View Scheme
Current Patent Assignee: GENENTECH - WO2015/52226, 2015, A1
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без приведенных структур исходников

1)Acetylaceton , Br2 bzw J2 ,Thioharnstoff;
Sarkis; Al-Azawe
[Journal of Chemical and Engineering Data, 1973, vol. 18, p. 99,100]

2)3-Chloroacetylaceton , Thioharnstoff;
Sarkis; Al-Azawe
[Journal of Chemical and Engineering Data, 1973, vol. 18, p. 99,100]

[paramona]

Спасибо, mishka!