HRID544440

反应详情

EQUATION

反应方程式

HRID 544440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3.3 g of (1R,3R) 2,2-dimethyl-3-(2,2-dibromoethenyl)-cyclopropane-1-carboxylic acid, 2.2 g of the product of Step A, 1.5 g of potassium carbonate, 100 mg of 1,4,7,10,13,16-hexaoxacyclooctadecane and 50 ml of methyl ethyl ketone wasrefluxed for 24 hours and was evaporated to dryness under reduced pressure.The residue was added to water and the aqueous mixture was extracted with ethyl acetate. The organic phase was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution withbenzene yielded 2.84 g of [5-phenoxy-(1,2,4)-thiadiazol-3-yl]-methyl (1R,3R) 2,2-dimethyl-3-(2,2-dibromoethenyl)-cyclopropane-1-carboxylate.

WORKUP

后处理

  1. customwas evaporated to dryness under reduced pressure
  2. additionThe residue was added to water
  3. extractionthe aqueous mixture was extracted with ethyl acetate
  4. customThe organic phase was evaporated to dryness under reduced pressure
  5. customthe residue was chromatographed over silica gel
  6. washElution withbenzene