反应 #2075723

反应方程式

2,4,6-Trichloro-5-methoxypyrimidine

ammonia

water

→

title compound

收率 88.0%

2,6-Dichloro-5-methoxy-pyrimidin-4-ylamine

收率 88.0%

溶剂

dimethyl sulfoxide

反应条件

后处理

1. 1
   其他3,984,411 for preparation)
2. 2
   过滤the precipitated product was collected by filtration
3. 3
   洗涤washed with water
4. 4
   workup.DISSOLUTIONThis solid was dissolved in 40 mL ethyl acetate
5. 5
   洗涤washed twice with water
6. 6
   洗涤washed once with brine
7. 7
   其他dried
8. 8
   其他evaporated

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.: 1HNMR (DMSO-d6+D2O) δ 3.71 (s, 3H).

来源