三乙胺 → 4-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

HRID 1591663笔记

反应方程式

HRID 1591663 反应方程式
ClC([O:4][C:5]([Cl:8])(Cl)Cl)=O.[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][NH:16][CH2:17][CH2:18][O:19][CH3:20])=[CH:13][CH:12]=1.C(N(CC)CC)C>ClCCl>[CH3:9][O:10][C:11]1[CH:22]=[CH:21][C:14]([CH2:15][N:16]([CH2:17][CH2:18][O:19][CH3:20])[C:5]([Cl:8])=[O:4])=[CH:13][CH:12]=1

参与物

5

反应物 3

HCID 8471三乙胺HCID 10426氯甲酸三氯甲酯HCID 3285873(4-甲氧基苄基)(2-甲氧基乙基)胺

产物 1

HCID 219560334-Methoxybenzyl(2-methoxyethyl)carbamoyl chloride

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

0.51 g (0.31 ml, 2.56 mmol) of trichloromethyl chloroformate (“diphosgene”) are dissolved in 15 ml of dichloromethane, and 1.00 g (5.12 mmol) of 4-methoxybenzyl(2-methoxyethyl)amine and 0.78 g (7.68 mmol) of triethylamine are slowly added. After stirring at room temperature overnight, the mixture is poured into ice-water and extracted three times with dichloromethane, and the organic phase is dried over magnesium sulfate and concentrated to dryness in a rotary evaporator. The crude product is employed without workup directly in the next stage.

后处理

  1. extractionextracted three times with dichloromethane
  2. dry with materialthe organic phase is dried over magnesium sulfate
  3. concentrationconcentrated to dryness in a rotary evaporator

来源与证据

ORD记录
ord-dd832533dd2d43deb4e651745db78f28
来源数据集
uspto-grants-2007_11
专利号
US07291622B2

反应笔记

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