醋酸 → 3-甲氧基-4-羟基苯乙腈

HRID 1576875

反应方程式

HRID 1576875 反应方程式
CN[CH2:3][C:4]1[CH:12]=[CH:11][C:9]([OH:10])=[C:6]([O:7][CH3:8])[CH:5]=1.[C-:13]#[N:14].[Na+].C(O)(=O)C>CS(C)=O.O>[OH:10][C:9]1[CH:11]=[CH:12][C:4]([CH2:3][C:13]#[N:14])=[CH:5][C:6]=1[O:7][CH3:8]

参与物

6

反应物 3

HCID 176醋酸HCID 8929氰化钠HCID 70607242-Methoxy-4-((methylamino)methyl)phenol

产物 1

HCID 782203-甲氧基-4-羟基苯乙腈

试剂、催化剂与溶剂 2

HCID 679二甲基亚砜溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
125 °C

实验过程

160.8 g of N-methylvanillylamine and 54 g of sodium cyanide are suspended in 1 liter of dimethylsulphoxide and dissolved by heating to 125°C. At this temperature, a solution of 100 ml of glacial acetic acid in 200 ml of water is added and the mixture is stirred for a further 2 hours under nitrogen at 125°C. It then cooled to 80°C and the dimethylsulphoxide is distilled off in a water-pump vacuum. 900 ml of water are added to the residue which is extracted with 350 ml of chloroform. The chloroform phase is extracted by shaking with water and dried with sodium sulphate. On distilling off the chloroform in vacuo, an oil is obtained, which is cooled and seeded. The crystals formed melt at 53°-54°C (boiling point0.1 :140°-144°C). The yield is 143 g (94% of theory).

后处理

  1. dissolutiondissolved
  2. temperatureIt then cooled to 80°C
  3. distillationthe dimethylsulphoxide is distilled off in a water-pump vacuum
  4. addition900 ml of water are added to the residue which
  5. extractionis extracted with 350 ml of chloroform
  6. extractionThe chloroform phase is extracted
  7. stirringby shaking with water
  8. dry with materialdried with sodium sulphate
  9. distillationOn distilling off the chloroform in vacuo
  10. customan oil is obtained
  11. temperaturewhich is cooled
  12. customThe crystals formed
  13. custommelt at 53°-54°C
  14. custom(boiling point0.1 :140°-144°C)

来源与证据

ORD记录
ord-cf0952bb1b0b45c9a0f3002a03677194
来源数据集
uspto-grants-1976_09
专利号
US03983151

关联笔记

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