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2,3-二甲基马来酸酐 → N-(5-tert-butyl-1,3,4-thiadiazol-2-yl)-2,3-dimethylmaleinimide

HRID 1761805
笔记
打印预览

反应方程式

HRID 1761805 反应方程式
[NH2:1][C:2]1[S:3][C:4]([C:7]([CH3:10])([CH3:9])[CH3:8])=[N:5][N:6]=1.[CH3:11][C:12]1[C:13]([O:15][C:16](=O)[C:17]=1[CH3:18])=[O:14]>C(O)(=O)C>[C:7]([C:4]1[S:3][C:2]([N:1]2[C:13](=[O:14])[C:12]([CH3:11])=[C:17]([CH3:18])[C:16]2=[O:15])=[N:6][N:5]=1)([CH3:10])([CH3:9])[CH3:8]
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 130102,3-二甲基马来酸酐HCID 1701702-氨基-5-叔丁基- 1,3,4-噻二唑

产物 1

HCID 14461005N-(5-tert-butyl-1,3,4-thiadiazol-2-yl)-2,3-dimethylmaleinimide收率 91%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂2 次

实验过程

2-Amino-5-tert-butyl-1,3,4-thiadiazole (1.57 g) and 2,3-dimethylmaleic anhydride (1.51 g) were refluxed for 5 hours in glacial acetic acid (30 ml). After the reaction, acetic acid and the excess of the 2,3-dimethylmaleic anhydride were evaporated. The residue was dissolved in dichloromethane (50 ml), and the solution was washed with a 10% aqueous solution of potassium carbonate (20 ml), and dried over anhydrous magnesium sulfate. The solvent was evaporated to give the desired N-(5-tert-butyl-1,3,4-thiadiazol-2-yl)-2,3-dimethyl-maleinimide (2.41 g). mp. 87°-91° C.

后处理

  1. customthe excess of the 2,3-dimethylmaleic anhydride were evaporated
  2. dissolutionThe residue was dissolved in dichloromethane (50 ml)
  3. washthe solution was washed with a 10% aqueous solution of potassium carbonate (20 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated

来源与证据

ORD记录
ord-0dab09b7878c46fbb05c832b91f5713f
来源数据集
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04828604

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记