Dimethyl Disulfide → (2-Chloro-6-fluorophenyl)(methyl)sulfane

温度

-78 °C

n-Butylithium (2.5M in hexane, 129 ml) was added to a solution of 3-fluorochlorobenzene (35 g) in dry tetrahydrofuran while maintaining the temperature below -70° C. The mixture was stirred at -78° C. for 3 hours and dimethyl disulphide (60.65 g) was added. The mixture was allowed to warm to room temperature and stirred overnight. The mixture was evaporated to dryness and the residue was suspended in ether and washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 2-chloro-6-fluorothioanisole (60 g) as a crude yellow oil containing some dimethyl disulphide, NMR (CDCl3) 2.45(s,3H), 6.95(t,1H), 7.1-7.3(m,2H).

1. temperaturewhile maintaining the temperature below -70° C
2. temperatureto warm to room temperature
3. stirringstirred overnight
4. customThe mixture was evaporated to dryness
5. washwashed with water
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customThe filtrate was evaporated to dryness

ORDレコード

ord-74d29cbdb4b64b6a9fac27f6d8a4488d

出典データセット

uspto-grants-1999_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05856274