Potassium Carbonate → 2-(4-Chloro-4,4-difluorobutylthio)thiazole

Solid anhydrous potassium carbonate (9.33 g) was added in two portions to a stirred mixture of 2-mercaptothiazole (7.90 g), 1,4-dichloro- 1,1-difluorobutane (9.70 g) and acetone (150 ml) under a nitrogen atmosphere, and the resultant mixture heated at the reflux temperature for 4 hours. After cooling to the ambient temperature the solid component was removed by filtration and washed with acetone (2×50 ml) and the combined washings and filtrate concentrated by evaporation of the solvent under reduced pressure. Diethyl ether (150 ml) was added to the residue and the resultant solution washed with aqueous potassium carbonate solution (2×100 ml) and with water (100 ml). After drying over anhydrous magnesium sulfate the solution was concentrated by removal of the solvent by evaporation under reduced pressure to yield 2-(4-chloro-4,4-difluorobutylthio)thiazole (13.98 g, 94%).

1. customwas removed by filtration
2. washwashed with acetone (2×50 ml)
3. concentrationthe combined washings and filtrate concentrated by evaporation of the solvent under reduced pressure
4. additionDiethyl ether (150 ml) was added to the residue
5. washthe resultant solution washed with aqueous potassium carbonate solution (2×100 ml) and with water (100 ml)
6. dry with materialAfter drying over anhydrous magnesium sulfate the solution
7. concentrationwas concentrated by removal of the solvent by evaporation under reduced pressure

ORDレコード

ord-ecc3ae2925bb4b71b5cfdde22c4cb0d4

出典データセット

uspto-grants-2000_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06025497