Hexane → (4-Bromo-2,6-dichlorophenyl)(trimethyl)silane

The 2,6-Dichloro-4-bromoiodobenzene (4.48 g, 12.7 mmol) was dissolved in diethyl ether (50 ml). To the solution was then added dropwise a hexane solution of n-butyl lithium (1.56 M, 8.2 ml) at −78° C. At the same temperature, the mixture was then stirred for 1 hour. To the mixture was then added dropwise trimethylsilyl trifluoromethanesulfonate (3.2 ml, 16.5 mmol). The mixture was then stirred at −78° C. for 1 hour and at room temperature for 30 minutes. After the quenching of the reaction with water, the mixture was then extracted with ether. The resulting organic phase was then dried over magnesium sulfate. The solvent was then distilled off. The crude product thus obtained was then distilled under reduced pressure in a glass tube oven so that it was purified to obtain 3,5-dichloro-4-trimethylsilyl-bromobenzene (3.39 g; yield: 90%).

1. stirringThe mixture was then stirred at −78° C. for 1 hour and at room temperature for 30 minutes
2. customAfter the quenching of the reaction with water
3. extractionthe mixture was then extracted with ether
4. dry with materialThe resulting organic phase was then dried over magnesium sulfate
5. distillationThe solvent was then distilled off
6. customThe crude product thus obtained
7. distillationwas then distilled under reduced pressure in a glass tube oven so that it
8. customwas purified

ORDレコード

ord-659b6c0f088d4756b4a3d2c014389226

出典データセット

uspto-grants-2007_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07189790B2