HRID50535

反应详情

EQUATION

反应方程式

HRID 50535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of trans-{4-[(naphthalene-1-sulfonylamino)-methyl]-cyclohexylmethyl}-carbamic acid tert-butyl ester (25 g) in chloroform (300 ml) is treated with a 4 N HCl solution in dioxane (300 ml) at 0° C. After completion, the reaction mixture is concentrated in vacuo, the residue is taken up in a 1 N sodium hydroxide solution and dichloromethane. After extraction with dichloromethane, the organics are dried over sodium sulfate and concentrated to 18.5 g of trans-naphthalene-1-sulfonic acid (4-aminomethyl-cyclohexylmethyl) -amide as a white powder melting at 157-162° C. Rf(C3) 0.36.

WORKUP

后处理

  1. concentrationAfter completion, the reaction mixture is concentrated in vacuo
  2. extractionAfter extraction with dichloromethane
  3. dry with materialthe organics are dried over sodium sulfate
  4. concentrationconcentrated to 18.5 g of trans-naphthalene-1-sulfonic acid (4-aminomethyl-cyclohexylmethyl) -amide as a white powder melting at 157-162° C