HRID1084626
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionTo a mixture of 2,2,6,6
- extractionextracted with aqueous 5% K2CO3
- extractionextracted with ether
- customThe combined organic layers are dried
- customevaporated
- customto give light yellow crystals, which
- customare purified
- customto yield 2,2,6,6