Acetic Acid → HCID 54385620、化合物

HRID 128743

反応式

HRID 128743 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 54385620HCID 54385620、化合物収率 14.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f0a802d59c9c4788a1516338c94a138d
出典データセット
uspto-grants-1995_11
特許番号
US05464856

関連ノート

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