HRID1684523

反应详情

EQUATION

反应方程式

HRID 1684523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.2 ml of 6N hydrochloric acid, 0.55 ml of trifluoroacetic acid and 2.38 g (8.8 mmol) of mercury(II)-chloride are successively added to a solution of 1.1 g (2.2 mol) of 7-benzyl-8-(3-(1,3-dithian-2-ylidene)-cyclopentyl)-1,3-dipropylpurine-2,6-dione in 30 ml of methanol and 6 ml of dichloromethane. The mixture is stirred for 4 hours at ambient temperature and then suction filtered over Celite. At -5° C., 90 mg of sodium borohydride are carefully added the filtrate, which is stirred for 30 minutes at 0° C., suction filtered over Celite and evaporated down. For purification the residue remaining is chromatographed on silica gel with a mixture of dichloromethane/methanol in the ratio 97:3. 0.72 g (72% of theory) of the title compound are obtained as a brownish oil.

WORKUP

后处理

  1. filtrationsuction filtered over Celite
  2. additionAt -5° C., 90 mg of sodium borohydride are carefully added the filtrate, which
  3. stirringis stirred for 30 minutes at 0° C.
  4. filtrationsuction filtered over Celite
  5. customevaporated down
  6. customFor purification the residue
  7. customremaining is chromatographed on silica gel with a mixture of dichloromethane/methanol in the ratio 97:3