Chlorotrimethylsilane → HCID 178478089、化合物

温度

0 °C

Under an argon stream, to a suspension of zinc powder (55.1 g, 843 mmol) in tetrahydrofuran (THF; 56 ml) was added 1,2-dibromoethane (2.9 ml, 33.8 mmol), and the mixture was heated under reflux for 5 min. Subsequently, trimethylsilyl chloride (8.6 ml, 67.5 mmol) was added at 0° C., and the mixture was stirred at 0° C. for 5 min. A solution of 2,3-dichlorobenzyl chloride (82.4 g, 421.7 mmol) in THF (330 ml) was added dropwise under ice-cooling, and after the completion of the dropwise addition, the mixture was allowed to warm to room temperature. The mixture was stirred for 1 hr to give a solution of 2,3-dichlorobenzylzinc chloride in THF.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 5 min
3. temperaturecooling
4. additionafter the completion of the dropwise addition
5. temperatureto warm to room temperature
6. stirringThe mixture was stirred for 1 hr

ORDレコード

ord-5a39f8bed747478d9d0d131a61047aa0

出典データセット

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07531554B2