تفاعل #45719

معادلة التفاعل

6-(Bromoacetyl)-2-(dimethylamino)-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile

thioacetamide

cesium carbonate

→

solid

المردود 79.0%

2-(Dimethylamino)-7-fluoro-5-methyl-6-(2-methyl-1,3-thiazol-4-yl)-1,3-benzoxazole-4-carbonitrile

المردود 79.0%

المذيبات

toluene

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   غسيلwashed with water
3. 3
   تجفيفdried over anhydrous sodium sulfate
4. 4
   أخرىThe solvent was evaporated away under reduced pressure
5. 5
   أخرىthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1 to 1:1)

الإجراء التجريبي

6-(Bromoacetyl)-2-(dimethylamino)-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile (I-170) (0.60 g, 1.76 mmol) was dissolved in toluene (30 ml), then thioacetamide (0.16 g, 2.13 mmol) and cesium carbonate (0.75 g, 2.30 mmol) were added, followed by stirring at an external temperature of 100° C. for 16 hours. The reaction liquid was diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1 to 1:1) to obtain a yellow solid (0.44 g, 79%).

المصدر