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Toluene → Ethyl allyl(2,2-dimethoxyethyl)carbamate

HRID 345795
ノート
印刷プレビュー

反応式

HRID 345795 の反応式
[H-].[Na+].[C:3]1([CH3:9])[CH:8]=CC=CC=1.[CH3:10][O:11][CH:12]([O:20][CH3:21])[CH2:13][NH:14][C:15](=[O:19])[O:16][CH2:17][CH3:18].C(Br)C=C>O>[CH2:9]([N:14]([CH2:13][CH:12]([O:11][CH3:10])[O:20][CH3:21])[C:15](=[O:19])[O:16][CH2:17][CH3:18])[CH:3]=[CH2:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1140TolueneHCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 10921057Ethyl 2,2-dimethoxyethylcarbamate

生成物 1

HCID 10943907Ethyl allyl(2,2-dimethoxyethyl)carbamate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

20 g of sodium hydride (80% strength in paraffin oil) are initially introduced into 500 ml of toluene and 89 g (0.5 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate are added dropwise at 80° C. The mixture is stirred at 80° C. for one hour and 73 g (0.6 mol) of allyl bromide are then added dropwise in the course of three hours. The mixture is stirred at 80° C. overnight, the salts are dissolved with water and the organic phase is separated off. The aqueous phase is extracted with toluene, the organic phases are dried over potassium carbonate and concentrated and the residue is distilled.

後処理

  1. additionare added dropwise at 80° C
  2. stirringThe mixture is stirred at 80° C. overnight
  3. customthe organic phase is separated off
  4. extractionThe aqueous phase is extracted with toluene
  5. dry with materialthe organic phases are dried over potassium carbonate
  6. concentrationconcentrated
  7. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-cf20850c7e40415d88270a1b22aabd7e
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05059597

反応ノート

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