4-Chlorobenzotrichloride → 3,4-Dichlorophenyltrichloromethane

温度

70 °C

In this apparatus, a mixture of 1,725 g (7.5 moles) of 4-chlorobenzotrichloride and 12 g (0.075 mole) of FeCl3 was heated to 70° C. and circulated. The introduction of 585 g (8.25 moles) of chlorine gas was then started. (chlorine gas was fed in at a rate such that no chlorine was detectable in the exit gas.) The reaction was complete after 5 hours. 2 liters of dilute hydrochloric acid were added to the reaction mixture and the organic phase was separated off, washed twice with 2 liters of water and dried over CaCl2. Subsequent fractional distillation gave 1,824 g of 3,4-dichlorobenzotrichloride (92% of theory) (98% purity according to a gas chromatogram), of boiling point 138°-140° C. at 12 mbar.

1. customthe organic phase was separated off
2. washwashed twice with 2 liters of water
3. dry with materialdried over CaCl2
4. distillationSubsequent fractional distillation

ORDレコード

ord-7b5fe7f8da4e4d218aa780c77a7ecd7d

出典データセット

uspto-grants-1988_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04769503