HRID2169302

反应详情

EQUATION

反应方程式

HRID 2169302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of (Z)-(1-amino-2-{8-phenyl-1,4-dioxaspiro[4.5]decan-8-yl}ethylidene)amino acetate (267) (1.4 g, 4.21 mmol) in methanol was added Pd—C (10%) under nitrogen atmosphere and the mixture was kept under a hydrogen atmosphere of balloon pressure at room temperature for 2 h (reaction was monitored by LC-MS). The reaction mixture was filtered and the filtrate was concentrated in vacuo to get a sticky mass which was triturated with diethyl ether to get pure 2-(8-phenyl-1,4-dioxa-spiro[4.5]dec-8-yl)acetamidine acetic acid salt (268) (1.25 g, 88.79%) as a white solid.

WORKUP

后处理

  1. custom(reaction was monitored by LC-MS)
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto get a sticky mass which
  5. customwas triturated with diethyl ether