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Acetic Anhydride → 5-[(3-Methoxyphenyl)methylene]-1-methyl-2,4-imidazolidinedione

HRID 128742
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인쇄 미리보기

반응식

HRID 128742 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1C=O.[CH3:11][N:12]1[CH2:18][C:16](=[O:17])[NH:15][C:13]1=[O:14].[C:19]([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O.C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:7]([CH:19]=[C:18]2[N:12]([CH3:11])[C:13](=[O:14])[NH:15][C:16]2=[O:17])[CH:8]=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 86582-MethoxybenzaldehydeHCID 692171-MethylhydantoinHCID 517045Sodium Acetate

생성물 1

HCID 544632705-[(3-Methoxyphenyl)methylene]-1-methyl-2,4-imidazolidinedione수율 18.2%

시약·촉매·용매 2

HCID 176Acetic Acid
용매
HCID 962Water용매

실험 절차

A mixture of 2-methoxybenzaldehyde (3.8 g, 28 mmoles), 1-methyl hydantoin (3.0 g 26 mmoles), sodium acetate (8.4 g, 102 mmoles), acetic anhydride (10 ml), and acetic acid (40 ml) is stirred under an inert atmosphere and heated to reflux. After 24 hours the mixture is stirred into water (350 ml), stirred, and the resulting gum is isolated and washed by decantation, then crystallized from isopropanol. Recrystallization from acetonitrile gave the pure product (1.1 g), mp 195°-197° C.

후처리

  1. temperatureheated to reflux
  2. stirringstirred
  3. customthe resulting gum is isolated
  4. washwashed by decantation
  5. customcrystallized from isopropanol
  6. customRecrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-73efcc85ea824ec8ab3eb3c2f8ac4619
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05464856

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