Diethyl Ether → HCID 20255641、化合物

A solution (about 100 mL) of 3,4-dichlorophenylmagnesium bromide in diethyl ether was prepared from a mixture of magnesium (flakes) (2.07 g) in diethyl ether (100 mL) and 1-bromo-3,4-dichlorobenzene (17.5 g). A solution of methoxyacetonitrile (5.0 g) in diethyl ether (10 mL) was added dropwise to a solution of 3,4-dichlorophenylmagnesium bromide in diethyl ether under ice-cooling, and the resulting mixture was stirred under ice-cooling for 20 min. The reaction mixture was quenched with water, the mixture was acidified with 1 N hydrochloric acid, and the mixture was stirred under ice-cooling for 15 min. The reaction mixture was extracted with ethyl acetate, the organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated to give a pale-yellow oil. The oil was purified by silica gel column chromatography (eluent; hexane:ethyl acetate (19:1-1:1)) to give the title compound (10.5 g).

1. temperaturecooling
2. temperaturecooling for 20 min
3. customThe reaction mixture was quenched with water
4. stirringthe mixture was stirred under ice-
5. temperaturecooling for 15 min
6. extractionThe reaction mixture was extracted with ethyl acetate
7. washthe organic layer was washed with water and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. customthe solvent was evaporated
10. customto give a pale-yellow oil
11. customThe oil was purified by silica gel column chromatography (eluent; hexane:ethyl acetate (19:1-1:1))

ORDレコード

ord-b6a355e289e34e41aa931d4762177826

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08722662B2