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

HRID 1199865

反応式

HRID 1199865 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 197340602-Methylbutyl 4-(4'-carbobenzoxyoxybenzoyloxy)benzoate収率 63%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-c451ceebfc764dc88c729636dff54986
出典データセット
uspto-grants-1990_02
特許番号
US04904065

関連ノート

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