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 by following the procedure described for Example-108 using 2-[(2-chloro-6-fluorophenyl)amino]-7,7-dimethyl-7,8-dihydro-1H-furo[3,2-e]benzimidazole-5-carboxylic acid (Intermediate-15, 0.100 g, 0.266 mmol), thionyl chloride (2.0 mL), 6-(difluoromethoxy)pyridin-3-amine (Intermediate-36, 0.065 g, 0.399 mmol), THF (5.0 mL) and DIPEA (2 mL). The obtained crude product was purified by column chromatography on basic alumina eluting with 0.7-1.0% MeOH:DCM to afford 0.020 g of the desired product. 1HNMR (DMSO-d6): δ 1.57 (s, 6H), 3.09 (s, 2H), 7.12 (d, J=8.7 Hz, 1H), 7.30-7.46 (m, 4H), 7.66 (s, 1H), 7.90 (s, 1H), 8.23 (d, J=9.0 Hz, 1H), 8.59 (s, 1H), 9.79 (s, 1H), 11.20 (s, 1H); MS [M+H]+: 518.24.
WORKUP
后处理
- customThe title compound was prepared
- customThe obtained crude product
- customwas purified by column chromatography on basic alumina eluting with 0.7-1.0% MeOH