Катализатор Граббса I поколения без PhCHN2

[Magic Methyl]

Коллеги, здравствуйте
Нужен катализатор Граббса I поколения. Хотел сделать самостоятельно. Исходники - cHex3P, RuCl3*H2O, стирол
есть под рукой. Посмотрел методики, - есть варианты без фенилдиазометана. Буду очень признателен, если
поделитесь рабочим методом его приготовления.
p/s. катализатора нужно 200-500 мг, на один-два эксперимента. Думал купить, но официально конечно же не
интересно, слишком долго ждать, а на складе такие штуки никто не держит как правило. Если методики
слишком сложно воспроизводимые, обращусь в соответствующий раздел, может быть кто то поделиться.
С уважением

[Magic Methyl]

Что скажет публика по поводу вот такого способа (Method for preparing ruthenium-carbene compound, CN114149467A)?:

"10.0g (38.2mmol) of RuCl3 The trihydrate was added to 60mL of THF and the reaction was run with H2 Displacement, followed by addition of 32.1g (115mmol) of tricyclohexylphosphine (PCy)3) And 10mL of 1-hexene. H is to be 2 (H2?) The pressure was increased to 1.05 atm and the reaction was stirred at 50 ℃ for 10 h. The resulting dark red liquid was cooled to 30 ℃. 7.80g (76.4mmol) phenylacetylene were added to the reaction by syringe and stirring was continued for 2 h. At this point 39.8g (382mmol) of styrene were added and the mixture was stirred for 1h at 60 ℃. Most of the reaction solvent is removed, ice methanol is added for pulping, a large amount of purple crystals appear, at the moment, filtration is carried out, and the filter cake is washed by the ice methanol until the washing liquid is basically colorless. The filter cake was dried under vacuum at room temperature to give 28.8g (91.5%) of a purple solid"

Выглядит просто, но химию данного процесса я не понимаю
С уважением

[tsarapoid]

что водород присобачивается к рутению, а потом замещается на карбен?
ну это реакции комплексных соединений переходных металлов
(в принципе там известно всего три элементарных акта)
reference https://patents.google.com/patent/CN114149467A/en

[tsarapoid]

Что скажет публика по поводу вот такого способа (Method for preparing ruthenium-carbene compound, CN114149467A)?:

proper translation from Chinese:

Example 3: Synthesis of Grubbs 1st generation catalyst
10.0 g (38.2 mmol) of RuCl₃ trihydrate was added to 60 mL of THF. The reaction system was purged with H₂, followed by the addition of 32.1 g (115 mmol) of tricyclohexylphosphine (PCy₃) and 10 mL of 1-hexene. The H₂ pressure was increased to 1.05 atmospheres, and the reaction was stirred at 50°C for 10 h. The resulting dark red liquid was cooled to 30°C. 7.80 g (76.4 mmol) of phenylacetylene was added via syringe to the reaction mixture and stirring continued for 2 h. Then, 39.8 g (382 mmol) of styrene was added, and the temperature was raised to 60°C and stirred for 1 h. Most of the reaction solvent was removed, and icy methanol was added to slurry the mixture. A large amount of purple crystals appeared, which were then filtered and the filter cake was rinsed with icy methanol until the rinse was essentially colorless. The filter cake was dried under vacuum at room temperature to yield 28.8 g (91.5%) of a purple solid. The purple solid is a Grubbs first generation catalyst, 31P NMR: δ 35.70 ppm (as shown in Figure 3). The structural formula is as follows: