Water → 1-Bromo-2-chloro-3-(methylsulfanyl)benzene

温度

-78 °C

To a solution of 1,3-dibromo-2-chlorobenzene (3.4 g, 12.6 mmol) in dry diethyl ether (60 ml), under nitrogen, at −78° C., was added dropwise n-butyllithium (2.5 M in hexane, 5.0 ml, 12.6 mmol). The mixture was stirred for 1 h after which dimethyldisulfide (1.0 ml, 13.9 mmol) was added dropwise. The resulting mixture was stirred at −78° C. for 30 min and then brought to ambient temperature. Water (100 ml) was added and the mixture was extracted with ethylacetate (3×100 ml). The combined organic phases was dried (MgSO4), filtered and evaporated to dryness.

1. additionwas added dropwise
2. custombrought to ambient temperature
3. extractionthe mixture was extracted with ethylacetate (3×100 ml)
4. dry with materialThe combined organic phases was dried (MgSO4)
5. filtrationfiltered
6. customevaporated to dryness

ORDレコード

ord-2be7e372087e462b94b5717c2d8d2c8c

出典データセット

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08314126B2