反应详情

温度

80 °C

A mixture of 4-[5-(6-chloro-2-methyl-pyridin-3-yl)-2,3-dihydro-benzofuran-2-yl]-piperidine-1-carboxylic acid isopropyl ester (160 mg) and sodium methyl sulfide (84 mg) in N,N-dimtehylformamide (1.6 mL) is stirred for 4 h at 80° C. Three more portions of sodium methyl sulfide (28 mg each) are added over the course of two days while stirring the reaction mixture at 80° C. until completion of the reaction. The reaction mixture is diluted with ethyl acetate, washed with water and brine, and concentrated in vacuo. The crude product is used without further purification for the next reaction step. LC (method 6): tR=1.31 min; Mass spectrum (ESI+): m/z=427 [M+H]+.

1. stirringwhile stirring the reaction mixture at 80° C.
2. customuntil completion of the reaction
3. washwashed with water and brine
4. concentrationconcentrated in vacuo
5. customThe crude product is used without further purification for the next reaction step