HRID1170033

反应详情

EQUATION

反应方程式

HRID 1170033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (1) (10 g, 38 mmol) in 10 mL pyridine was added 6.6 g (47 mmol) of benzoyl chloride and stirred overnight at room temperature. The solution was evaporated under reduced pressure. The residue was dissolved in 1 M KOH and stirred for 3 h after which the Ph was adjusted to 2 with conc. HCl. The target compound (2) precipitated out. Yield: 9.3 g (90%). 1H NMR (d6-DMSO): δ 4.59 (s, 2 H, CH2O), 7.31 (d, 1 H, H5), 7.5-8.2 (7 H, aromatic, NH, H6). MS (FAB) m/z 273 (M+H)+ (calcd 273).

WORKUP

后处理

  1. customThe solution was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in 1 M KOH
  3. stirringstirred for 3 h after which the Ph
  4. customThe target compound (2) precipitated out