反応 #1042

反応方程式

3,4,4-trifluoro-3-butenoyl chloride

2-amino-4,6-dimethoxypyrimidine

potassium carbonate

→

title compound

収率 10.7%

2-(3,4,4-trifluoro-1-oxo-3-butenyl)amino-4,6-dimethoxy-pyrimidine

収率 10.7%

溶媒

dichloromethane

water

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred in cold for 10 min
2. 2
   洗浄The organic layer was washed with 3N HCl (2×25 mL), saturated sodium bicarbonate (25 mL) and brine
3. 3
   その他dried
4. 4
   その他Evaporation of the solvent

実験手順

To an ice-cooled stirred suspension of 2-amino-4,6-dimethoxypyrimidine (1.55 g, 10 mmol) in dichloromethane (50 mL) and potassium carbonate (2.76 g, 20 mmol) in water (20 mL) was added 3,4,4-trifluoro-3-butenoyl chloride (3.17 g, 20 mmol). The reaction mixture was stirred in cold for 10 min and at r.t. for 15 min. The organic layer was washed with 3N HCl (2×25 mL), saturated sodium bicarbonate (25 mL) and brine, and dried. Evaporation of the solvent gave 0.296 g (10%) of the title compound as a white solid. m.p. 127°-130° C.

出典