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. Then, trimethylsilyl chloride (8.6 ml, 67.5 mmol) was added at 0° C. and the mixture was stirred at 0° C. for 5 min, after which a solution of 2,3-dichlorobenzyl chloride (82.4 g, 421.7 mmol) in THF (330 ml) was added dropwise with ice-cooling. After completion of the dropwise addition, the mixture was warmed to room temperature and 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 completion of the dropwise addition
5. temperaturethe mixture was warmed to room temperature
6. stirringstirred for 1 hr

ORDレコード

ord-6c552893a17c45cd95cacf07d34e3298

出典データセット

uspto-grants-2007_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07176220B2