HRID249761

反应详情

EQUATION

反应方程式

HRID 249761 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-amino-7-benzyl-3,7-dihydro-6H-purin-6-one (25.0 g, 0.104 mol) in acetic acid (750.0 mL) and water (50.0 mL) at 55° C. was added a solution of sodium nitrite (28 g, 0.41 mol) in water (50 ml) dropwise. After the addition, the mixture was continued to stir for about 30 min until no starting material was left and then cooled to room temperature. The reaction mixture was concentrated to about ⅓ of its original volume, then diluted with 250 ml water. The precipitate formed was collected by filtration to provide the desired product (20 g, 79.7%). LCMS calculated for C12H11N4O2(M+H): 243.1. found: 243.1.

WORKUP

后处理

  1. additionAfter the addition
  2. waitwas left
  3. concentrationThe reaction mixture was concentrated to about ⅓ of its original volume
  4. additiondiluted with 250 ml water
  5. customThe precipitate formed
  6. filtrationwas collected by filtration