HRID1084626

反应详情

EQUATION

反应方程式

HRID 1084626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 2,2,6,6.tetramethyl.5.(4.chloro.2.nitrobenzoyloxy)-3,6-dihydro-2H-pyran-3-one (5.97 g, 16.9 mmol) and triethylamine (4,70 ml, 33.8 mmol) in 30 ml of acetonitrile is added acetone cyanohydrin (0.5 ml), and the mixture is stirred at RT for 24 hours. The reaction mixture is diluted with ether and extracted with aqueous 5% K2CO3. The aqueous layer is made acidic with conc. HCl and extracted with ether. The combined organic layers are dried and evaporated to give light yellow crystals, which are purified to yield 2,2,6,6.tetramethyl-4-(4-chloro-2-nitrobenzoyl) -2H-pyran-3,5-(4H,6H)-dione (compound 8, Table A).

WORKUP

后处理

  1. additionTo a mixture of 2,2,6,6
  2. extractionextracted with aqueous 5% K2CO3
  3. extractionextracted with ether
  4. customThe combined organic layers are dried
  5. customevaporated
  6. customto give light yellow crystals, which
  7. customare purified
  8. customto yield 2,2,6,6