HRID875100

反应详情

EQUATION

反应方程式

HRID 875100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate (1.00 g, 4 mmol) in anhydrous ethyl formate (10 mL) was treated with sodium ethoxide (0.54 g, 8 mmol) and refluxed for 3 hours. The mixture was cooled to room temperature and poured into cold water (40 mL). The aqueous layer was washed with diethyl ether (40 mL) to remove unreacted starting material, acidified with a 20% NaH2PO4 solution and extracted with ethyl acetate (50 mL×2). The organic extracts were collected, dried on Na2SO4 and evaporated to dryness to obtain the title compound (0.88 g, 78.8% yield) as a brown solid.

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. washThe aqueous layer was washed with diethyl ether (40 mL)
  3. customto remove unreacted
  4. extractionextracted with ethyl acetate (50 mL×2)
  5. customThe organic extracts were collected
  6. customdried on Na2SO4
  7. customevaporated to dryness