HRID1005

反应详情

EQUATION

反应方程式

HRID 1005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

27.3 g of 4-(1,4-dioxaspiro[4.5]dec-8-ylamino)-3-methoxy-2-methylpyridine hydrochloride are stirred with 400 ml of formic acid for 4 hours. The residue which remains after concentrating in vacuo is dissolved in methylene chloride and shaken with 2N NaOH. The methylene chloride phase is concentrated, the residue is dissolved in ether and the hydrochloride is precipitated by addition of ethereal HCl. 14 g=90%; m.p.: 115° to 120° C.

WORKUP

后处理

  1. concentrationafter concentrating in vacuo
  2. dissolutionis dissolved in methylene chloride
  3. concentrationThe methylene chloride phase is concentrated
  4. dissolutionthe residue is dissolved in ether
  5. customthe hydrochloride is precipitated by addition of ethereal HCl