甲胺-D5 → 2-(2,5-Dimethylthien-3-yl)-N-methylimidazo[2,1-b]-benzothiazole-3-acetamide

HRID 36912笔记

反应方程式

HRID 36912 反应方程式
[CH3:1][C:2]1[S:3][C:4]([CH3:23])=[CH:5][C:6]=1[C:7]1[N:8]=[C:9]2[N:13]([C:14]=1[CH2:15][C:16]([OH:18])=O)[C:12]1[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=1[S:10]2.[CH3:24][NH2:25]>O1CCCC1>[CH3:1][C:2]1[S:3][C:4]([CH3:23])=[CH:5][C:6]=1[C:7]1[N:8]=[C:9]2[N:13]([C:14]=1[CH2:15][C:16]([NH:25][CH3:24])=[O:18])[C:12]1[CH:19]=[CH:20][CH:21]=[CH:22][C:11]=1[S:10]2

参与物

4

反应物 2

HCID 6329甲胺-D5HCID 199367062-(2,5-Dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetic acid

产物 1

HCID 199367242-(2,5-Dimethylthien-3-yl)-N-methylimidazo[2,1-b]-benzothiazole-3-acetamide

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

反应条件

温度
0 °C

实验过程

A solution of 1.5 g (0.0044 mole) of 2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetic acid in 30 ml of anhydrous tetrahydrofuran is treated, at room temperature, with 0.85 g (0.005 mole) of N,N'-carbonyldiimidazole for 30 minutes. The solution which has become clear is cooled to 0° C. and a stream of methylamine is passed through it for 30 minutes. The mixture is allowed to return to room temperature, the stirring is continued for 3 h, the solvent is evaporated under reduced pressure, the residue is taken up in 10 ml of water, it is extracted with dichloromethane, the organic phase is separated, it is washed with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure, and the residue is crystallized from ethyl acetate. 1 g of pale yellow crystals is finally obtained. Melting point: 238°-239° C.

后处理

  1. customto return to room temperature
  2. customthe solvent is evaporated under reduced pressure
  3. extractionit is extracted with dichloromethane
  4. customthe organic phase is separated
  5. washit is washed with water, it
  6. dry with materialis dried over sodium sulphate
  7. customthe solvent is evaporated under reduced pressure
  8. customthe residue is crystallized from ethyl acetate

来源与证据

ORD记录
ord-7156c0337bdd40d492d7eeed097f1fac
来源数据集
uspto-grants-1995_05
专利号
US05418248

反应笔记

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