HRID627283
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A solution of (S,E)-tert-butyl (2,2,3,3,11,11,12,12-octamethyl-7-methylene-4,10-dioxa-3,11-disilatridecan-6-yl)(2-oxopent-3-en-1-yl)carbamate (Intermediate 279, 10 g, 18.45 mmol) in toluene (400 mL) was purged with nitrogen for 15 minutes. The Hoveyda-Grubbs Catalyst 2nd Generation (2.320 g, 3.69 mmol) was then added. The reaction was heated at 100° C. overnight. Another 0.05 eq of catalyst was added and the reaction mixture was heated at 100° C. for another 2 hours. The reaction mixture was concentrated onto silica gel. Silica gel chromatography (0%-15% ethyl acetate/hexanes) afforded the title compound (8.55 g, 93%) as a light brown oil.
WORKUP
后处理
- temperaturethe reaction mixture was heated at 100° C. for another 2 hours
- concentrationThe reaction mixture was concentrated onto silica gel