Diethyl Ether → 2-Methylbutyl 4-(4'-carbobenzoxyoxybenzoyloxy)benzoate

HRID 231012

反応式

HRID 231012 の反応式
[CH3:1][CH:2]([CH2:14][CH3:15])[CH2:3][O:4][C:5](=[O:13])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.[C:16]([O:26][C:27]1[CH:35]=[CH:34][C:30]([C:31](Cl)=[O:32])=[CH:29][CH:28]=1)([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17].CCOCC>C1COCC1.N1C=CC=CC=1>[CH3:1][CH:2]([CH2:14][CH3:15])[CH2:3][O:4][C:5](=[O:13])[C:6]1[CH:7]=[CH:8][C:9]([O:12][C:31](=[O:32])[C:30]2[CH:29]=[CH:28][C:27]([O:26][C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])=[CH:35][CH:34]=2)=[CH:10][CH:11]=1

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 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 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 16 m moles(3.3 g) of the above 4-hydroxybenzoic acid 2-methylbutyl ester in 20 ml of THF and 40 ml of pyridine was cooled, and a THF solution of 10 m moles(2.9 g) of the above 4-carbobenzoxyoxybenzoyl chloride was added dropwise. The mixture was returned slowly to room temperature, then stirred for 8 hours. After the reaction, the reaction mixture was ether extracted and concentrated, and then purified by column chromatography to obtain 2.9 g of 4-(4'-carbobenzoxyoxybenzoyloxy)benzoic acid 2-methylbutyl ester [m.p. 64.4°-65.4° C⟧ (yield: 63%)

後処理

  1. customwas returned slowly to room temperature
  2. customAfter the reaction
  3. extractionextracted
  4. concentrationconcentrated
  5. custompurified by column chromatography

出典と根拠

ORDレコード
ord-9ae0164c134f4c678979543892b72d2a
出典データセット
uspto-grants-1989_07
特許番号
US04844835

関連ノート

読み込み中…