HRID1445340

反应详情

EQUATION

反应方程式

HRID 1445340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

1.12 g of N-benzyl-3-hydroxy-thiophene-2-carboxamide, 3.16 g of 4,5-diacetoxy-6-acetoxymethyl-2-bromo-tetrahydro-pyran-3-yl acetate, 3.30 g of potassium carbonate and 235 mg of benzyltributylammonium chloride were dissolved in 25 ml of dichloromethane, and 2.00 ml of water were added. The reaction mixture was stirred at 22° C. for 40 h. 50 ml of saturated sodium bicarbonate solution were added to the reaction mixture, which was extracted twice with 50 ml of dichloromethane each time. The combined organic phases were dried over magnesium sulfate and concentrated. The crude product was purified by column chromatography (SiO2, ethyl acetate/n-heptane=1:1).

WORKUP

后处理

  1. extractionwas extracted twice with 50 ml of dichloromethane each time
  2. dry with materialThe combined organic phases were dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe crude product was purified by column chromatography (SiO2, ethyl acetate/n-heptane=1:1)