HRID1898341
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of methyl 4,5-diamino-2-hydroxybenzoate (0.500 g, 2.74 mmol) in acetonitrile (15.0 mL) was added 1,3-dichloro-2-isothiocyanatobenzene (Intermediate-5, 0.550 g, 2.72 mmol). The reaction mass was stirred at RT for 24 h and N,N-di-isopropyl carbodimide (1.0 mL) was added to it. The reaction mass stirred at RT for 4-6 h. The reaction mass was cooled and filtered to afford 0.500 g of the desired product. 1HNMR (DMSO-d6): δ 3.86 (s, 3H), 6.56 (s, 1H), 7.22 (t, J=7.8 Hz, 1H), 7.38 (s, 1H), 7.52 (d, J=7.8 Hz, 2H), 10.49-10.64 (s, 3H); MS [M+H]+: 352.08.
WORKUP
后处理
- stirringThe reaction mass stirred at RT for 4-6 h
- temperatureThe reaction mass was cooled
- filtrationfiltered