HRID1755871

反应详情

EQUATION

反应方程式

HRID 1755871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

N-[[5-(Benzyloxy)-3,4-dihydro-3-methyl-4-oxo-2-pyrimidinyl]methoxy]phthalimide (1.56 g) (4 mmol) are dissolved in 110 ml of dichloromethane and treated dropwise at about -70° C. while stirring with 0.42 ml (4.4 mmol) of boron tribromide. After stirring at about -70° C. for 4 hours and at room temperature for 16 hours the solvent is removed in a water-jet vacuum at room temperature. The residue is treated with about 30 ml of water, the insoluble product is filtered off and washed firstly with water and subsequently with diethyl ether. After drying in a high vacuum at room temperature for 18 hours there are obtained 1.1 g of N-[(3,4-dihydro-5-hydroxy-3-methyl-4-oxo-2-pyrimidinyl)methoxy]phthalimide as a white powder, m.p. 172° C. (dec.).

WORKUP

后处理

  1. additiontreated dropwise at about -70° C.
  2. customis removed in a water-jet vacuum at room temperature
  3. additionThe residue is treated with about 30 ml of water
  4. filtrationthe insoluble product is filtered off
  5. washwashed firstly with water and subsequently with diethyl ether
  6. customAfter drying in a high vacuum at room temperature for 18 hours there