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Water → methyl N-(5-bromomethyl-2-chlorobenzyl)carbamate

HRID 2414262
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인쇄 미리보기

반응식

HRID 2414262 반응식
[Cl:1][C:2]1[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][C:3]=1[CH2:4][NH:5][C:6](=[O:9])[O:7][CH3:8].P(Br)(Br)[Br:17].O.C(OCC)(=O)C>COCCOC>[Br:17][CH2:14][C:11]1[CH:12]=[CH:13][C:2]([Cl:1])=[C:3]([CH:10]=1)[CH2:4][NH:5][C:6](=[O:9])[O:7][CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 24614Phosphorus tribromideHCID 22645125methyl N-(2-chloro-5-hydroxymethylbenzyl)carbamate

생성물 1

HCID 22645123methyl N-(5-bromomethyl-2-chlorobenzyl)carbamate수율 209%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane
용매

실험 절차

6.2 g of methyl N-(2-chloro-5-hydroxymethylbenzyl)carbamate was dissolved in 50 ml of ethylene glycol dimethyl ether, and 2.7 g of phosphorus tribromide was dropwise added to this solution at −20° C., followed by stirring at room temperature for 1 hour. After completion of the reaction, water was added to the reaction solution, extraction with ethyl acetate was carried out, followed by washing with an aqueous sodium hydrogencarbonate solution, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.1 g of methyl N-(5-bromomethyl-2-chlorobenzyl)carbamate as white crystals.

후처리

  1. washby washing with an aqueous sodium hydrogencarbonate solution
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-37e4f85fd98944f39e6f909f7c23875f
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06812229B1

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