HRID380465

反应详情

EQUATION

反应方程式

HRID 380465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.19 g (0.47 mmol) of 1-allyloxycarbamoyl-3-(SR)-(4-phenylpiperidinylmethyl)-4-(RS)-(3-thienyl)pyrrolidine, 0.52 g (9.4 mmol) KOH and 0.23 mL (4.7 mmol) of hydrazine hydrate in 5 mL of ethylene glycol was heated at 140° C. for 12 h. The reaction mixture was cooled to rt and diluted with ether. The reaction mixture was washed 3 times with H2O, dried over Na2SO4, filtered and the filtrate was concentrated to give 0.13 g of the title compound. 1H NMR (CDCl3) δ7.22-7.37 (m, 7H), 7.04 (d, 1H, J=4.3 Hz), 3.32-3.39 (m, 2H), Mass Spectrum (CI) m/e=327 (M+1).

WORKUP

后处理

  1. washThe reaction mixture was washed 3 times with H2O
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated