Réaction #2075723

Équation de réaction

2,4,6-Trichloro-5-methoxypyrimidine

ammonia

water

→

title compound

Rendement 88.0%

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

Rendement 88.0%

Solvants

dimethyl sulfoxide

Conditions de réaction

Traitement

1. 1
   Autre3,984,411 for preparation)
2. 2
   Filtrationthe precipitated product was collected by filtration
3. 3
   Lavagewashed with water
4. 4
   workup.DISSOLUTIONThis solid was dissolved in 40 mL ethyl acetate
5. 5
   Lavagewashed twice with water
6. 6
   Lavagewashed once with brine
7. 7
   Autredried
8. 8
   Autreevaporated

Mode opératoire

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).

Source