HRID846846

反应详情

EQUATION

反应方程式

HRID 846846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-6,8-dichloropurine (2.04 g), 6,6-dimethyl-5,7-dioxaspiro[2.5]octane-4,8-dione (1.73 g) and anhydrous potassium carbonate (2.12 g) in N,N-dimethylformamide (40 ml) was stirred at room temperature for 18 hours under dry nitrogen. The solvent was evaporated and the residue dissolved in water (60 ml) and acidified from pH 10 to pH 4 with dilute hydrochloric acid. The yellow precipitate was filtered off, washed with water and dried to give 2-amino-6,8-dichloro-9-[1-(2,2-dimethyl-1,3-dioxane4,6-dione-5-yl)eth-2-yl]purine (2.2 g, 50%). T.1.c. r.f. 0.65 (25% methanol-dichloromethane).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in water (60 ml)
  3. filtrationThe yellow precipitate was filtered off
  4. washwashed with water
  5. customdried