Hydrochloric Acid → 4-Chloro-3-(hydroxymethyl)phenol

HRID 657837

反応式

HRID 657837 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:9]=1[C:10](O)=[O:11].Cl>O1CCCC1.O.O1CCCC1>[Cl:7][C:8]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][C:9]=1[CH2:10][OH:11]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4582102-Chloro-5-hydroxybenzoic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 247215304-Chloro-3-(hydroxymethyl)phenol

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 21881883Oxolane--water (1/1)溶媒

実験手順

Lithium aluminium hydride (1M in diethyl ether, 25 mL, 25 mmol) was added to an ice-cooled solution of 2-chloro-5-hydroxy-benzoic acid (4 g, 23.2 mmol) in tetrahydrofuran (200 mL) and the mixture was heated under reflux for 6 hours. The mixture was then diluted with a mixture of water/tetrahydrofuran, acidified with 1M hydrochloric acid, and extracted with ethyl acetate. The organic solution was dried over sodium sulphate and concentrated in vacuo to afford the title compound in quantitative yield, 4.3 g.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 6 hours
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic solution was dried over sodium sulphate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9d324e7d830b4262a401a8f0f3f35f71
出典データセット
uspto-grants-2011_12
特許番号
US08076356B2

関連ノート

読み込み中…