Methanol → 3(2,2-Dichlorovinyloxy)benzyl alcohol

温度

60 °C

A mixture 3(2,2-dichlorovinyloxy)benzyl bromide (2.8 g), sodium p-toluene sulphonate (2.0 g) and methanol (20 ml) is warmed to 50°C for 1 hour, after which water (20 ml) and toluene (20 ml) is added with agitation. The toluene layer is separated, washed with water and concentrated by evaporation of the solvent under reduced pressure. The concentrate is then added dropwise to a 15% (w/v) aqueous solution of potassium hydroxide (100 ml) and the mixture warmed to 60°C for 1 hour, cooled to the ambient temperature and extracted with a mixture of toluene (10 ml) and methyl iso-butylketone (10 ml), the extracts dried over anhydrous magnesium sulphate and the solvents evaporated under reduced pressure to yield 3(2,2-dichlorovinyloxy)benzyl alcohol as a residual pale yellow oil.

1. customThe toluene layer is separated
2. washwashed with water
3. concentrationconcentrated by evaporation of the solvent under reduced pressure
4. additionThe concentrate is then added dropwise to a 15% (w/v) aqueous solution of potassium hydroxide (100 ml)
5. temperaturecooled to the ambient temperature
6. extractionextracted with a mixture of toluene (10 ml) and methyl iso-butylketone (10 ml)
7. dry with materialthe extracts dried over anhydrous magnesium sulphate
8. customthe solvents evaporated under reduced pressure

ORDレコード

ord-b971276c258d47b8a9598a4d28b968ea

出典データセット

uspto-grants-1976_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US03979519