Trimethyltin chloride → HCID 66609061、化合物

温度

-78 °C

A solution of (S)-2-(2-methylbutyl)thiophene (4.27 g, 27.7 mmol) in dry THF (100 mL) was cooled to −78° C., and a solution of n-BuLi (2.5 M, 16.6 mL, 41.5 mmol) was then added slowly. This mixture was stirred at −78° C. for additional 10 minutes, and then allowed to warm to room temperature and stirred at room temperature for 30 minutes, before it was cooled back to −78° C. A solution of trimethylstannyl chloride (1.0 M, 43 mL, 43.0 mmol) was added slowly. This mixture was stirred at −78° C. for 2 hours, and then allowed to warm to room temperature, and stirred at room temperature overnight. The reaction was quenched by water (20 mL), and the reaction mixture was diluted with hexane, washed with water, dried over Na2SO4, and concentrated on a rotary evaporator, leading to a slightly yellow oil (8.7 g, 99.1%), which was used directly in the next step without further purification.

1. temperatureto warm to room temperature
2. stirringstirred at room temperature for 30 minutes, before it
3. temperaturewas cooled back to −78° C
4. stirringThis mixture was stirred at −78° C. for 2 hours
5. temperatureto warm to room temperature
6. stirringstirred at room temperature overnight
7. customThe reaction was quenched by water (20 mL)
8. additionthe reaction mixture was diluted with hexane
9. washwashed with water
10. dry with materialdried over Na2SO4
11. concentrationconcentrated on a rotary evaporator
12. customwas used directly in the next step without further purification

ORDレコード

ord-b9a389090b62451c8395e3e153c3651f

出典データセット

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08598575B2