Succinic anhydride → HCID 15599091, 화합물

HRID 986799노트

반응식

HRID 986799 반응식
[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]

참가 물질

4

반응물 2

HCID 7922Succinic anhydride2회HCID 15599089HCID 15599089, 화합물

생성물 1

HCID 15599091HCID 15599091, 화합물수율 93.1%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0362687f58bb4b218961bc8e094fbf4b
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04716178

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