alpha-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride → N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide

HRID 36910笔记

反应方程式

HRID 36910 反应方程式
Cl.Cl[CH:3]([C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27])[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].C(S([O-])=O)O.[Na+]>ClCCl>[CH3:8][N:6]([CH3:7])[C:4](=[O:5])[CH2:3][C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27]

参与物

4

反应物 2

HCID 19936712alpha-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochlorideHCID 23689980次硫酸氢钠甲醛

产物 1

HCID 19936717N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

34 g (0.077 mole) of α-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 500 ml of dichloromethane are treated with 36.9 g (0.24 mole) of Rongalite®, while stirring the mixture at room temperature for 24 h. The organic phase is separated after settling has taken place, the solid residue is washed with dichloromethane, the organic phase is washed with a saturated sodium hydrogen carbonate solution and then with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure and 22 g of solid are obtained. After recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals are finally obtained. Melting point: 194°-195° C.

后处理

  1. customThe organic phase is separated after settling
  2. washthe solid residue is washed with dichloromethane
  3. washthe organic phase is washed with a saturated sodium hydrogen carbonate solution
  4. dry with materialwith water, it is dried over sodium sulphate
  5. customthe solvent is evaporated under reduced pressure and 22 g of solid
  6. customare obtained
  7. customAfter recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
  8. customare finally obtained

来源与证据

ORD记录
ord-d92df32fa3c24976935b2b186cc36c14
来源数据集
uspto-grants-1995_05
专利号
US05418248

反应笔记

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