Succinic anhydride → HCID 15599091、化合物

HRID 986799ノート

反応式

HRID 986799 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH2:3][CH2:2]1.[NH:8]([C:15]1[CH:20]=[C:19]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:18]([OH:25])=[C:17]([C:26]([CH3:29])([CH3:28])[CH3:27])[CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>COCCOC>[C:21]([C:19]1[CH:20]=[C:15]([CH:16]=[C:17]([C:26]([CH3:29])([CH3:28])[CH3:27])[C:18]=1[OH:25])[N:8]([C:4](=[O:5])[CH2:3][CH2:2][C:1]([OH:6])=[O:7])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([CH3:24])([CH3:23])[CH3:22]

参加物

4

反応物 2

HCID 7922Succinic anhydride2 回HCID 15599089HCID 15599089、化合物

生成物 1

HCID 15599091HCID 15599091、化合物収率 93.1%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

1.5 g (0.015 mole) of succinic anhydride, 4.5 g (0.010 mole) of 4-anilino-2,6-di-t-butylphenol, and 10 ml of 1,2-dimethoxyethane were combined and heated at reflux for 48 hours. 1.5 g of succinic anhydride and 5 ml of 1,2-dimethoxyethane were added and the reaction was heated for an additional 24 hours. The reaction mixture was cooled in an ice bath. The resulting precipitate was collected, rinsed with a small amount of cold 1,2-dimethoxyethane, and recrystallized from a mixture of ethanol and water to give 3.7 g of off-white 4-(3,5-di-t-butyl-4-hydroxy-N-phenylanilino)-4-oxobutanoic acid, m.p. 205°-208° C. Analysis: Calculated for C24H31NO4 : % C, 72.5; % H, 7.9; % N, 3.5: Found: % C, 72.4; % H, 7.8; % N, 3.3.

後処理

  1. temperatureheated
  2. temperatureat reflux for 48 hours
  3. temperaturethe reaction was heated for an additional 24 hours
  4. temperatureThe reaction mixture was cooled in an ice bath
  5. customThe resulting precipitate was collected
  6. washrinsed with a small amount of cold 1,2-dimethoxyethane
  7. customrecrystallized from a mixture of ethanol and water

出典と根拠

ORDレコード
ord-0362687f58bb4b218961bc8e094fbf4b
出典データセット
uspto-grants-1987_12
特許番号
US04716178

反応ノート

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