间苯二胺 → HCID 22883495，化合物

HRID 2256

反应方程式

HRID 2256 反应方程式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[C:3]([NH2:7])[CH:2]=1.[C:9]1(=[O:16])[O:15][C:13](=[O:14])[CH:12]=[C:10]1[CH3:11]>CC(C)=O>[C:1]1([NH:8][C:13](=[O:14])/[CH:12]=[C:10](/[CH3:11])\[C:9]([OH:16])=[O:15])[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:13](=[O:14])/[CH:12]=[C:10](/[CH3:11])\[C:9]([OH:15])=[O:16])[CH:2]=1

参与物

4

反应物 2

HCID 7935间苯二胺HCID 12012柠康酸酐

产物 1

HCID 22883495HCID 22883495，化合物收率 99.9%

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂3 次

实验过程

A 3-liter, 3-neck round bottom flask was charged with 54 g (0.5 mole) of m-phenylenediamine and 500 ml of reagent acetone and flushed with nitrogen. The flask was fitted with a reflux condenser, mechanical stirrer and thermocouple. A dropping funnel containing 112 g (1.0 mole) of citraconic anhydride in 500 ml of reagent acetone was attached and the solution added dropwise over about 1 1/2 hours with stirring as the temperature was allowed to rise to reflux the acetone. The reaction mixture was refluxed for an additional hour, cooled to room temperature and suction filtered to give 166 g of N,N'-(m-phenylene)bis citraconamic acid as shown by NMR analysis, as a tan mustard-colored solid melting at 152°-156° C.

后处理

  1. customflushed with nitrogen
  2. customThe flask was fitted with a reflux condenser, mechanical stirrer
  3. additionthe solution added dropwise over about 1 1/2 hours
  4. temperatureThe reaction mixture was refluxed for an additional hour
  5. filtrationsuction filtered

来源与证据

ORD记录
ord-81e816ae13fd471baa1f76ede4d59949
来源数据集
uspto-grants-1998_03
专利号
US05728757

关联笔记

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