HRID864989

反应详情

EQUATION

反应方程式

HRID 864989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of dimethyl 2-(2-amino-6-chloropurin-9-ylmethyl)succinate (3.28 g, 10 mmol), sodium acetate (1.5 g) and 5% palladium on charcoal (0.4 g) in ethanol (200 ml) was hydrogenated with agitation in a Parr apparatus at 40 psi for 115 h/room temperature. After filtration, sodium acetate (1.6 g) and 5% Pd/C (0.4 g) were added and the hydrogenation was continued for 70 h. After filtration and evaporation to dryness, the residue was extracted with 2×50 ml of chloroform and the combined extracts were evaporated to dryness affording 2.6 g (89%) of crude dechlorinated product.

WORKUP

后处理

  1. customroom temperature
  2. filtrationAfter filtration, sodium acetate (1.6 g) and 5% Pd/C (0.4 g)
  3. additionwere added
  4. waitthe hydrogenation was continued for 70 h
  5. filtrationAfter filtration and evaporation to dryness
  6. extractionthe residue was extracted with 2×50 ml of chloroform
  7. customthe combined extracts were evaporated to dryness
  8. customaffording 2.6 g (89%) of crude dechlorinated product