반응 #2075723

반응 방정식

2,4,6-Trichloro-5-methoxypyrimidine

ammonia

water

→

title compound

수율 88.0%

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

수율 88.0%

용매

dimethyl sulfoxide

반응 조건

후처리

1. 1
   기타3,984,411 for preparation)
2. 2
   여과the precipitated product was collected by filtration
3. 3
   세척washed with water
4. 4
   workup.DISSOLUTIONThis solid was dissolved in 40 mL ethyl acetate
5. 5
   세척washed twice with water
6. 6
   세척washed once with brine
7. 7
   기타dried
8. 8
   기타evaporated

실험 절차

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).

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