反应详情

A solution of 5-[2-(2,2,2-trifluoroethyl)guanidino]-3-[2-(3-cyano-2-methylisothioureido)ethylthiomethyl]-1,2,4-thiadiazole in 33% w/v methylamine in ethanol (4 ml.) was kept at 20° for 18 hours. Volatile material was evaporated in vacuo and the crude material was fractionated on a silica column (26 cm.×1 cm. diameter) eluted with a methanol/ethyl acetate 1:50 v/v to give 5-[2-(2,2,2-trifluoroethyl)guanidino]-3-[2-(2-cyano-3-methylguanidino)ethylthiomethyl]-1,2,4-thiadiazole. The n.m.r. spectrum in d6 dimethylsulphoxide using tetramethyl silane as an internal standard (δ=0) had the following resonances (δ): 4.2 (2H, quartet); 3.8 (2H, singlet); 3.3 (2H, multiplet); 2.7 (2H, triplet).

1. customVolatile material was evaporated in vacuo
2. washeluted with a methanol/ethyl acetate 1:50 v/v