Hydrochloric Acid → 4-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid-tert-butylamide

HRID 1656898

反応式

HRID 1656898 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6385Tert-ButylamineHCID 150095674-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid chloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f615a415704b4d12a7d5dae619e84c9f
出典データセット
uspto-grants-1993_10
特許番号
US05256633

関連ノート

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