HRID1252343

反应详情

EQUATION

反应方程式

HRID 1252343 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 0.2 gram (0.0007 mole) of 1-(4-chloro-2-fluoro-5-hydroxyphenyl)-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one, 0.3 gram (0.0007 mole) of N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-bromopropionamide, 0.3 gram (0.002 mole) of potassium carbonate in 20 ml of acetone was heated under reflux for 18 hours. The reaction mixture was cooled and concentrated under reduced pressure to a residue. The residue was dissolved in 100 ml of water and the solution acidified by the dropwise addition of concentrated hydrochloric acid. The resultant precipitate was collected by filtration, washed with water, and dried to yield N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionamide; m.p. 198°-201° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperatureThe reaction mixture was cooled
  4. concentrationconcentrated under reduced pressure to a residue
  5. dissolutionThe residue was dissolved in 100 ml of water
  6. additionthe solution acidified by the dropwise addition of concentrated hydrochloric acid
  7. filtrationThe resultant precipitate was collected by filtration
  8. washwashed with water
  9. customdried