Hydrochloric Acid → 2,6-Dichloro-4-(2,2,2-trifluoroethylthio)-phenol

64 g of potassium carbonate were added to a solution of 41.9 g of 3,5-dichloro-4-hydroxy-benzenethiol in 200 ml of N,N-dimethylformamide under nitrogen atmosphere. To the stirred mixture were dropped at 30° to 40° C. 55 g of 2,2,2-trifluoroethyl-benzenesulfonate. The whole was stirred at 60° to 70° C. for 6 hours, cooled, mixed with 1.5 l of water, and acidified to pH 2 by dropwise addition of hydrochloric acid. A resulted oil was extracted with toluene and the toluene extract was washed with water. The washed toluene extracted was stirred with 160 ml of a 25% aqueous potassium hydroxide solution, and a water layer was separated. Then the separated water layer was acidified to pH 2 by adding hydrochloric acid. A resulted oil was extracted with toluene. The toluene extract was washed with water, dried over anhydrous sodium sulphate, and evaporated to give a residue. The residue was distilled under reduced pressure to give 42.3 g of 2,6 -dichloro-4-(2,2,2-trifluoroethylthio)-phenol which boiled at 85° to 88° C./1 mmHg.

1. additionTo the stirred mixture were dropped at 30° to 40° C
2. temperaturecooled
3. extractionA resulted oil was extracted with toluene
4. extractionthe toluene extract
5. washwas washed with water
6. extractionThe washed toluene extracted
7. stirringwas stirred with 160 ml of a 25% aqueous potassium hydroxide solution
8. customa water layer was separated
9. additionby adding hydrochloric acid
10. extractionA resulted oil was extracted with toluene
11. extractionThe toluene extract
12. washwas washed with water
13. dry with materialdried over anhydrous sodium sulphate
14. customevaporated
15. customto give a residue
16. distillationThe residue was distilled under reduced pressure

ORDレコード

ord-652e40a41dca4bd3b4ebcabd297aa1e2

出典データセット

uspto-grants-1986_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04609669