反应 #1489174
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09156798B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 3-ethoxy-2,2-dimethylcyclobutanamine (1.0 equiv.) and 4-chloro-2-(methylthio)pyrimidine-5-carbonitrile (1.1 equiv.) in tert-butanol/1,2-dichloroethane (0.5 M) was treated with potassium carbonate powder (3.0 equiv.). The resulting reaction mixture was then heated at 70° C. under nitrogen for 3 h. After cooling, ethyl acetate was added and the mixture was vigorously stirred. The solid was removed by vacuum-filtration. The filtrate was concentrated and further dried to give (100% yield) of waxy, yellow solid, which was used in the next step without further purification. MS (ESI) m/z 293.0 [M+1]+. The resulting reaction mixture After cooling The solid was removed by vacuum-filtration The filtrate was concentrated further dried to give (100% yield) of waxy, yellow solid, which was used in the next step without further purification
来源 ID: ord-faf4807f230e43769abb6eaa025388a4