HRID1675757
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
A solution of [3-(2-methoxy-2-oxoethyl)-4,6-dimethyl-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl]acetic acid (Intermediate 9) (305 mg, 1.04 mmol), N,N-dimethylamine hydrochloride (128 mg, 1.60 mmol), EDC (300 mg, 1.60 mmol), HOBT (240 mg, 1.60 mmol), and N, N-diisopropylethylamine (0.909 mL, 5.20 mmol) were stirred for 16 h at ambient temperature in DMF (3 mL). The mixture was partitioned between CH2Cl2 (10 mL) and saturated NaHCO3 (10 mL) and the organic layer was dried over Na2SO4, filtered, and concentrated to give the compound. MS: m/z=320 (M+1).
WORKUP
后处理
- customThe mixture was partitioned between CH2Cl2 (10 mL) and saturated NaHCO3 (10 mL)
- dry with materialthe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customto give the compound