HRID1912299

反应详情

EQUATION

反应方程式

HRID 1912299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4,6-Trichloro-5-methoxypyrimidine (1.0 g, 4.7 mmol, see U.S. Pat. No. 3,984,411 for preparation) was dissolved in 15 mL dry dimethyl sulfoxide (DMSO) and treated with a stream of ammonia gas for 30 min. The mixture was poured into 30 mL water and the precipitated product was collected by filtration and washed with water. This solid was dissolved in 40 mL ethyl acetate, washed twice with water, washed once with brine, dried and evaporated to give the title compound (800 mg, 88% yield): mp 155-156° C.: 1H NMR (DMSO-d6+D2O) δ 3.71 (s, 3H).

WORKUP

后处理

  1. custom3,984,411 for preparation)
  2. filtrationthe precipitated product was collected by filtration
  3. washwashed with water
  4. dissolutionThis solid was dissolved in 40 mL ethyl acetate
  5. washwashed twice with water
  6. washwashed once with brine
  7. customdried
  8. customevaporated