海萝胶 → 4-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid-tert-butylamide

HRID 5333

反应方程式

HRID 5333 反应方程式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([S:14][CH3:15])[S:9][C:10]=1[C:11](Cl)=[O:12])=[O:5])[CH3:2].[C:16]([NH2:20])([CH3:19])([CH3:18])[CH3:17].Cl>ClCCl>[C:16]([NH:20][C:11]([C:10]1[S:9][C:8]([S:14][CH3:15])=[N:7][C:6]=1[C:4]([O:3][CH2:1][CH3:2])=[O:5])=[O:12])([CH3:19])([CH3:18])[CH3:17]

参与物

5

反应物 3

HCID 313海萝胶HCID 6385LY3295668HCID 150095674-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid chloride

产物 1

HCID 150095734-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid-tert-butylamide收率 100.2%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

3.50 g (13.2 mmol) of 4-ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid chloride was dissolved in 20 ml of dichloromethane and dripped, at 0° C., into a solution of 3.20 g (44 mmol) of tert-butylamine in 50 ml of dichloromethane. The mixture was allowed to warm up to room temperature and was then stirred for 14 hours. 100 ml of 10% strength hydrochloric acid was added and the organic phase was separated, washed with 50 ml of water and dried over sodium sulfate. The solvent was removed under reduced pressure, leaving 4.00 g (100%) of product as a yellow crystalline slurry.

后处理

  1. customthe organic phase was separated
  2. washwashed with 50 ml of water
  3. dry with materialdried over sodium sulfate
  4. customThe solvent was removed under reduced pressure

来源与证据

ORD记录
ord-e8d6c976acfe418eb1c313ed305dfb2d
来源数据集
uspto-grants-1993_09
专利号
US05244867

关联笔记

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