Water → 4-Hydroxybenzyl cyanide

HRID 262429

반응식

HRID 262429 반응식
O.[OH:2][C:3]1[CH:13]=[CH:12][C:6]([CH:7](O)[C:8]([O-])=O)=[CH:5][CH:4]=1.[Na+].[Cl-].[Na+].[C-]#[N:18].[Na+].O>CN(C)C=O.C(O)=O>[OH:2][C:3]1[CH:13]=[CH:12][C:6]([CH2:7][C:8]#[N:18])=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 5234Sodium ChlorideHCID 8929Sodium CyanideHCID 236981332-Hydroxy-2-(4-hydroxyphenyl)acetic acid, sodium salt hydrate

생성물 1

HCID 265484-Hydroxybenzyl cyanide

시약·촉매·용매 2

HCID 284Formic Acid용매HCID 6228Dimethylformamide용매

반응 조건

온도
135 °C

실험 절차

A stirred suspension of sodium p-hydroxymandelate monohydrate (50 g. of 77% w/w material, the impurity being sodium chloride) and sodium cyanide (12.5 g.) in N,N-dimethylformamide (67.5 ml.) is heated at 135° C. for 2 hours and then cooled. Water (200 ml.) and formic acid (20 ml.) are added and the mixture is extracted twice with methyl isobutyl ketone (200 ml. and 100 ml.). The combined extracts are washed twice with water (50 ml. each time) and are then concentrated by evaporation. There is thus obtained a solution of p-hydroxybenzyl cyanide in methyl isobutyl ketone which is suitable for conversion to p-hydroxyphenylacetamide without further purification.

후처리

  1. temperaturecooled
  2. extractionthe mixture is extracted twice with methyl isobutyl ketone (200 ml. and 100 ml.)
  3. washThe combined extracts are washed twice with water (50 ml
  4. concentrationeach time) and are then concentrated by evaporation

출처 및 근거

ORD 기록
ord-1413b00779fe4c989f620225bd258016
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154757

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