HRID1675757

反应详情

EQUATION

反应方程式

HRID 1675757 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe mixture was partitioned between CH2Cl2 (10 mL) and saturated NaHCO3 (10 mL)
  2. dry with materialthe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give the compound