4-Hydroxybenzyl Alcohol → 4-(3-tert-Butyl-4-methoxybenzoyloxymethyl)phenol

HRID 274039

反応式

HRID 274039 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][OH:9])=[CH:4][CH:3]=1.N1C=CC=CC=1.[C:16]([C:20]1[CH:21]=[C:22]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[C:23](Cl)=[O:24])([CH3:19])([CH3:18])[CH3:17].O>C1COCC1>[C:16]([C:20]1[CH:21]=[C:22]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[C:23]([O:9][CH2:8][C:5]1[CH:6]=[CH:7][C:2]([OH:1])=[CH:3][CH:4]=1)=[O:24])([CH3:19])([CH3:17])[CH3:18]

参加物

6

反応物 4

HCID 1254-Hydroxybenzyl AlcoholHCID 962WaterHCID 1049PyridineHCID 136335553-Tert-butyl-4-methoxybenzoyl chloride

生成物 1

HCID 214745304-(3-tert-Butyl-4-methoxybenzoyloxymethyl)phenol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1.24 g (0.01 mol) of 4-hydroxybenzenemethanol, 1 ml (0.01 mol) of pyridine and 50 ml of THF are introduced into a round-bottomed flask. While cooling in an icebath, a solution of 2.2 g (0.01 mol) of 3-tert-butyl-4-methoxybenzoyl chloride in 50 ml of THF is introduced dropwise and the mixture is stirred at room temperature for 24 h. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column and eluted with a mixture of dichloromethane and ethyl ether (97:3).

後処理

  1. temperatureWhile cooling in an icebath
  2. extractionthe mixture is extracted with ethyl ether
  3. customthe organic phase is separated after settling
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customThe residue obtained
  7. customis purified by chromatography on a silica column
  8. washeluted with a mixture of dichloromethane and ethyl ether (97:3)

出典と根拠

ORDレコード
ord-6f43e7ba229e4366a2732b9a84ac901f
出典データセット
uspto-grants-1995_02
特許番号
US05387594

関連ノート

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