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

HRID 345795
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인쇄 미리보기

반응식

HRID 345795 반응식
[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]
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참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cf20850c7e40415d88270a1b22aabd7e
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05059597

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