HRID1898453
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
The title compound was prepared following the procedure described for Example-177 using 7-[(2,6-dichlorophenyl)amino]-2-methyl-8H-imidazo[4,5-e][1,3]benzoxazole-4-carboxylic acid (Intermediate-55, 0.050 g, 0.132 mmol), oxalyl chloride (0.1 mL), 1-[2-(trifluoromethyl)phenyl]methanamine (0.046 g, 0.262 mmol), THF (5.0 mL) and 60% NaH (0.021 g, 0.525 mmol). The obtained crude product was purified by column chromatography on neutral alumina eluting with 1.5-2.0% MeOH:DCM to afford 0.027 g of the desired product. 1HNMR (DMSO-d6): δ 2.64 (s, 3H), 4.76 (s, 2H), 7.37-7.47 (m, 2H), 7.61-7.63 (m, 5H), 7.75 (d, J=6.9 Hz, 1H), 8.65 (s, 1H), 9.43 (s, 1H), 11.53 (s, 1H); MS [M+H]+: 534.43.
WORKUP
后处理
- customThe title compound was prepared
- customThe obtained crude product
- customwas purified by column chromatography on neutral alumina eluting with 1.5-2.0% MeOH