HRID508781

反应详情

EQUATION

反应方程式

HRID 508781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The title compound was prepared by following the procedure as described in step-2 of Intermediate-28 by using N-(4-chloro-3-nitrobenzyl)cyclopropanecarboxamide (0.400 g), methanol (10 mL), iron powder (catalytic) and conc.HCl (5 mL). The reaction mass was refluxed for 2 h. The reaction mass was quenched in water and basified with NaHCO3 and extracted with DCM. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 0.200 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 0.65 (d, J=8.4 Hz, 4H), 1.57 (m, 1H), 4.11 (d, J=5.4 Hz, 2H), 5.34 (s, 2H), 6.41 (d, J=7.2 Hz, 1H), 7.10 (d, J=7.8 Hz, 1H), 8.50 (br s, 1H); MS (m/z): 225.07 (M+H)+.

WORKUP

后处理

  1. customThe title compound was prepared
  2. temperatureThe reaction mass was refluxed for 2 h
  3. customThe reaction mass was quenched in water
  4. extractionextracted with DCM
  5. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  6. concentrationconcentrated