HRID1011013

反应详情

EQUATION

反应方程式

HRID 1011013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-dichloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine (3.08 g, containing triphenylphosphine oxide) was heated with 2M ammonia in IPA (50 mL) at 50° C., overnight. The reaction mixture was then evaporated to dryness to give a yellow solid. This material (3.2089 g) was recrystallised using methanol (50 mL) and after cooling the resultant solid was filtered and washed with methanol (5 mL) to give the title compound (1.5554 g). The filtrate was evaporated and recrystallised from methanol (25 mL) and after cooling the resultant solid was filtered to give a second crop (0.2324 g) and was consistent with first batch by NMR and LCMS.

WORKUP

后处理

  1. customThe reaction mixture was then evaporated to dryness
  2. customto give a yellow solid
  3. customThis material (3.2089 g) was recrystallised
  4. temperatureafter cooling the resultant solid
  5. filtrationwas filtered
  6. washwashed with methanol (5 mL)