HRID1931202
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of (4-Chloro-6-hydrazino-[1,3,5]triazin-2-yl)-(4-fluoro-3-trifluoromethylphenyl)-amine (XXIII) (264 mg, 1.38 mmol) in ethanol (8 mL) was added trifluoromethoxybenzaldehyde (200 mg, 0.694 mmol). The mixture was stirred overnight and filtered to give a white precipitate. The mother liquor was concentrated in vacuo and the residue recrystallized from ethyl acetate. The solids were combined and dried in vacuo to afford the titled compound 3 as white solid (123 mg, 38% yield): m.p. 185-186° C.; ESI/MS 461 (M+H), 459(M−H); 1H NMR (CDCl3): δ 8.5 (bs, 1H), 7.95 (s, 1H), 7.80 (m, 2H), 7.65 (m, 1H), 7.2-7.4, m, 6H).
WORKUP
后处理
- filtrationfiltered
- customto give a white precipitate
- concentrationThe mother liquor was concentrated in vacuo
- customthe residue recrystallized from ethyl acetate
- customdried in vacuo