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5-Chloro-2-methoxybenzoyl chloride → 4-(5-Chloro-2-methoxybenzamidomethyl)-phenylacetic acid

HRID 1277661
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인쇄 미리보기

반응식

HRID 1277661 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].Cl.[NH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][C:23]([OH:25])=[O:24])=[CH:18][CH:17]=1>CC(C)=O.[OH-].[Na+].O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7]([NH:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][C:23]([OH:25])=[O:24])=[CH:18][CH:17]=1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 123841765-Chloro-2-methoxybenzoyl chlorideHCID 53407881(4-(Aminomethyl)phenyl)acetic acid--hydrogen chloride (1/1)

생성물 1

HCID 234531114-(5-Chloro-2-methoxybenzamidomethyl)-phenylacetic acid수율 22.1%

시약·촉매·용매 3

HCID 180Acetone용매2회HCID 962Water용매
HCID 14798
Sodium Hydroxide
용매

실험 절차

A solution of 5.0 g 5-chloro-2-methoxybenzoyl chloride in 10 ml acetone is added, with ice cooling, to a solution of 5.0 g 4-aminomethyl-phenylacetic acid hydrochloride in 25 ml 2 N aqueous sodium hydroxide solution and 25 ml acetone. The reaction mixture is then stirred for 3 hours at ambient temperature, diluted with water, filtered with charcoal and the filtrate acidified with 2 N hydrochloric acid. The precipitate obtained is filtered off with suction and dried and then recrystallized from ethyl acetate/petroleum ether. There is obtained 1.8 g (21% of theory) 4-(5-chloro-2-methoxybenzamidomethyl)-phenylacetic acid; m.p. 140°-141° C.

후처리

  1. filtrationfiltered with charcoal
  2. customThe precipitate obtained
  3. filtrationis filtered off with suction
  4. customdried
  5. customrecrystallized from ethyl acetate/petroleum ether

출처 및 근거

ORD 기록
ord-8d4b4341943c42da9cdb35e26c8613be
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04278680

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