HRID384239
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
- 0 °C
PROCEDURE
实验过程
To a cooled (−70° C.) mixture of thiophene (17.6 g, 0.21 mol) in anhydrous THF (100 mL) was added dropwise a solution of n-BuLi (137.5 ml, 1.6 M, 0.22 mol) in hexane. After stirring for 1 hour at 0° C., the mixture was cooled to −40° C. followed by addition of 1-hexylbromide (0.22 mol). The mixture was slowly heated to r.t. Water (250 mL) was added and the mixture was extracted with diethylether (3×150 mL). The combined organic fractions were dried over MgSO4 and concentrated in vacuo. The product was purified by means of vacuum distillation. This product was prepared according to the general procedure and obtained as a colourless oil (26.5 g, 75%).
WORKUP
后处理
- temperatureTo a cooled
- temperaturethe mixture was cooled to −40° C.
- temperatureThe mixture was slowly heated to r.t
- extractionthe mixture was extracted with diethylether (3×150 mL)
- dry with materialThe combined organic fractions were dried over MgSO4
- concentrationconcentrated in vacuo
- distillationThe product was purified by means of vacuum distillation
- customThis product was prepared