Water → 4-Hydroxybenzyl cyanide

HRID 262429

反応式

HRID 262429 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 265484-Hydroxybenzyl cyanide

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
135 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1413b00779fe4c989f620225bd258016
出典データセット
uspto-grants-1979_05
特許番号
US04154757

関連ノート

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