HRID523131

反应详情

EQUATION

反应方程式

HRID 523131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirred solution of diethyl[(6-bromo-2-formylquinolin-7-yl)(difluoro)methyl]phosphonate (525 mg, 1.244 mmol) [Example 8, Step 4] in ethanol (12 mL) at room temperature were added hydroxylamine hydrochloride (130 mg, 1.865 mmol) and sodium acetate (508 mg, 3.73 mmol). The reaction mixture was stirred at 70° C. for 1 hour. It was then poured into aqueous sodium hydrogen carbonate and extracted with ethyl acetate (100 mL), washed with aqueous sodium hydrogen carbonate (2×), brine, dried with MgSO4, and concentrated in vacuo to give crude diethyl[(6-bromo-2-[(E)-(hydroxyimino)methyl]quinolin-7-yl)(difluoro)methyl]phosphonate.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (100 mL)
  2. washwashed with aqueous sodium hydrogen carbonate (2×), brine
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo