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Acetic Acid → 5-[(4-Hydroxy-3-methoxyphenyl)methylene]-1-methyl-2,4-imidazolidinedione

HRID 128743
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인쇄 미리보기

반응식

HRID 128743 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][C:3]=1[O:10][CH3:11].[CH3:12][N:13]1[CH2:19][C:17](=[O:18])[NH:16][C:14]1=[O:15].NCCC(O)=O.C(O)(=O)C>O>[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[C:19]2[N:13]([CH3:12])[C:14](=[O:15])[NH:16][C:17]2=[O:18])=[CH:4][C:3]=1[O:10][CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 239Beta-AlanineHCID 1183VanillinHCID 692171-Methylhydantoin

생성물 1

HCID 543856205-[(4-Hydroxy-3-methoxyphenyl)methylene]-1-methyl-2,4-imidazolidinedione수율 14.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

A mixture of 4-hydroxy-3-methoxybenzaldehyde (4.6 g, 30 mmoles), 1-methyl hydantoin (3.5 g, 30 mmoles), β-alanine (1.4 g, 16 mmoles), and acetic acid (40 ml) is stirred under an inert atmosphere and heated to reflux. After 8 hours the mixture is stirred into water (300 ml) and the precipitate filtered off, rinsed successively with water (3X), ethanol (2X), and ether (2X), and dried. Recrystallization from acetonitrile gave the pure product (1.1 g), mp 197°-198° C.

후처리

  1. temperatureheated to reflux
  2. filtrationthe precipitate filtered off
  3. washrinsed successively with water (3X), ethanol (2X), and ether (2X)
  4. customdried
  5. customRecrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-f0a802d59c9c4788a1516338c94a138d
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05464856

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