HRID908217

反应详情

EQUATION

反应方程式

HRID 908217 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-morpholin-4-yl-pyrimidine-4,6-diamine (1.0 g, 5.1 mmol), ω-bromoacetophenone (1.02 g, 5.1 mmol), NaHCO3 (473 mg, 6 mmol) and methanol (15 ml) was heated under an atmosphere of argon to reflux (3 h). After cooling, water (10 ml) was added (the gummy precipitate could not be isolated). Methanol was evaporated, the residue was taken up in ethyl acetate, washed (water), and dried (Na2SO4). The solvent was evaporated and the title compound (900 mg, 50%) was isolated from the mixture by column chromatography (silica gel, heptane:ethyl acetate=80:20-60:40). MS (m/e)=296.3 [M+H+].

WORKUP

后处理

  1. temperaturewas heated under an atmosphere of argon
  2. temperatureto reflux (3 h)
  3. temperatureAfter cooling
  4. custombe isolated)
  5. customMethanol was evaporated
  6. washwashed (water)
  7. dry with materialdried (Na2SO4)
  8. customThe solvent was evaporated