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

HRID 657837

반응식

HRID 657837 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 247215304-Chloro-3-(hydroxymethyl)phenol

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 21881883Oxolane--water (1/1)용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d324e7d830b4262a401a8f0f3f35f71
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076356B2

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