化工社
首页MCP工作台Skills
首页工作台通知我的
llms.txt · MCP 指南隐私政策 · 服务条款 · 支持v1.8.0
  1. 首页
  2. /反应

Methanol → HCID 70491208,化合物

HRID 463544
笔记
打印预览

反应方程式

HRID 463544 反应方程式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([NH:6]C)=[C:4]([N+:10]([O-])=O)[CH:3]=1.NN.[CH3:15]O>[Ni]>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH3:15])([NH2:6])[CH:4]([NH2:10])[CH:3]=1
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 887MethanolHCID 9321HydrazineHCID 27368364-氯-N-甲基-2-硝基苯胺

产物 1

HCID 70491208HCID 70491208,化合物收率 84%

试剂、催化剂与溶剂 1

HCID 935Nickel催化剂

实验过程

32.5 g (0.175M) of 4-Chloro-2-nitro-N-methylaniline of A above are added gradually to 24 g Raney-Nickel (wet) and 48 g hydrazine in methanol. A large amount of heat is generated. After the addition is complete, the solution is heated to reflux for 3 hours and filtered to remove the metal catalyst. The solvent is removed and the residue dissolved in methylene chloride. The methylene chloride solution is extracted with water and the mixture is filtered to remove the emulsion. The layers are separated and the methylene chloride layer is dried over anhydrous magnesium sulfate. After removal of the solvent, the residue is recrystallized from hexane. The substituted phenylenediamine weighs 22.6 g (84% yield) and has a melting point of 51°-2° C.

本页导航参与物实验过程后处理来源与证据反应笔记

后处理

  1. temperatureA large amount of heat
  2. additionAfter the addition
  3. temperaturethe solution is heated
  4. temperatureto reflux for 3 hours
  5. filtrationfiltered
  6. customto remove the metal catalyst
  7. customThe solvent is removed
  8. dissolutionthe residue dissolved in methylene chloride
  9. extractionThe methylene chloride solution is extracted with water
  10. filtrationthe mixture is filtered
  11. customto remove the emulsion
  12. customThe layers are separated
  13. dry with materialthe methylene chloride layer is dried over anhydrous magnesium sulfate
  14. customAfter removal of the solvent
  15. customthe residue is recrystallized from hexane

来源与证据

ORD记录
ord-53b572a1796d4a96928b78df2d499802
来源数据集
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04520196

反应笔记

加载中…