反应详情

温度

16 °C

Add triethylamine (234.5; mL, 1.68; mol) to a cooled suspension of 1-(5-amino-3-bromo-isothiazol-4-yl)-ethanone (310; g, 1.40; mol) in dichloromethane (2.79; L, 43.53 mol) at 0° C. under nitrogen and then add slowly a solution of cyclopropanecarbonyl chloride (137.5; mL, 1.47; mol) in dichloromethane (310; mL, 4.84; mol) at 0° C. over 1 hour. Warm to 16° C. over 2; hours and then cool to 10° C., add water (1; L) and separate the layers. Extract the aqueous layer once with dichloromethane (500; mL). Combine the organic layers, concentrate and purify by silica gel chromatography eluting with n-hexane:dichloromethane 30:70. Triturate the recovered solid with hexanes to give the title compound as a white solid (256.1; g, 60%). MS (m/z): 289, 291; (M+1).

1. temperaturehours and then cool to 10° C.
2. customseparate the layers
3. extractionExtract the aqueous layer once with dichloromethane (500; mL)
4. concentrationCombine the organic layers, concentrate
5. custompurify by silica gel chromatography
6. washeluting with n-hexane:dichloromethane 30:70
7. customTriturate the recovered solid with hexanes