反应详情

温度

120 °C

A mixture of 2-thiophenecarboxamide (5.09 g) and 1,3-dichloroacetone (457 g) was stirred at 120° C. for 2 hours. The reaction mixture was poured into water, nautralized with potassium carbonate, and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography. From the fraction eluted with diethyl ether-hexane (1:9, v/v), 4-chloromethyl-2-(2-thienyl)oxazole (4.09 g, 57%) was obtained. Recrystallization from isopropylether gave colorless needles, mp 59-59° C.

1. extractionextracted with ethyl acetate
2. washThe ethyl acetate layer was washed with water
3. dry with materialdried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. washFrom the fraction eluted with diethyl ether-hexane (1:9, v/v)