Pyridine → 2-Methylbutyl 4-(4'-carbobenzoxyoxybenzoyloxy)benzoate

HRID 1199865

반응식

HRID 1199865 반응식
[OH:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([O:8][CH2:9][CH:10]([CH3:13])[CH2:11][CH3:12])=[O:7])=[CH:4][CH:3]=1.N1C=CC=CC=1.[C:22]([O:32][C:33]1[CH:41]=[CH:40][C:36]([C:37](Cl)=[O:38])=[CH:35][CH:34]=1)([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23]>O1CCCC1>[C:22]([O:32][C:33]1[CH:34]=[CH:35][C:36]([C:37]([O:1][C:2]2[CH:3]=[CH:4][C:5]([C:6]([O:8][CH2:9][CH:10]([CH3:13])[CH2:11][CH3:12])=[O:7])=[CH:14][CH:15]=2)=[O:38])=[CH:40][CH:41]=1)([O:24][CH2:25][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)=[O:23]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 13530949Benzoic acid, 4-hydroxy-, 2-methylbutyl esterHCID 197340544-Carbobenzoxyoxybenzoyl chloride

생성물 1

HCID 197340602-Methylbutyl 4-(4'-carbobenzoxyoxybenzoyloxy)benzoate수율 63%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 16 mmol (3.3 g) of the 2-methylbutyl p-hydroxybenzoate obtained in 1.(2) in a solvent mixture of 20 ml of THF (tetrahydrofuran) and 40 ml of pyridine was cooled, and to the solution was added dropwise a THF solution of 10 mmol (2/9 g) of the 4-carbobenzoxyoxybenzoyl chloride obtained in 1.(4). The temperature was gradually returned to room temperature, and then the mixture was stirred for 8 hours. After conclusion of the reaction, the reaction solution and purified by column chromatography to obtain 2.9 g of 2-methylbutyl 4-(4'-carbobenzoxyoxybenzoyloxy)benzoate [m.p.: 64.4°-65.4° C⟧ (Yield: 63%)

후처리

  1. temperaturewas cooled
  2. customobtained in 1.(4)
  3. customwas gradually returned to room temperature
  4. customAfter conclusion of the reaction
  5. customthe reaction solution and purified by column chromatography

출처 및 근거

ORD 기록
ord-c451ceebfc764dc88c729636dff54986
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904065

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