Chloroacetone → Ethyl 4-methyl-1,3-thiazole-2-carboxylate

HRID 1889048

反応式

HRID 1889048 の反応式
[NH2:1][C:2](=[S:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl[CH2:10][C:11](=O)[CH3:12]>C(O)C>[CH3:12][C:11]1[N:1]=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[S:8][CH:10]=1

参加物

4

反応物 2

HCID 6571ChloroacetoneHCID 2733398Ethyl thiooxamate

生成物 1

HCID 567306Ethyl 4-methyl-1,3-thiazole-2-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl amino(thioxo)acetate (500 mg, 3.75 mmol) in ethanol (9.387 ml) was stirred at room temperature under an atmosphere of argon. 1-Chloro-2-propanone (0.299 ml, 3.75 mmol) was added and the solution was heated to reflux for 48 hours. The solution was allowed to cool to room temperature and then it was concentrated under reduced pressure to give a yellow coloured oily solid. The residue was chromatographed [SiO2, 0-100% EtOAc in Hexane] to give a yellow coloured oil identified as product in 208 mg.

後処理

  1. temperaturethe solution was heated
  2. temperatureto reflux for 48 hours
  3. concentrationit was concentrated under reduced pressure
  4. customto give a yellow coloured oily solid
  5. customThe residue was chromatographed [SiO2, 0-100% EtOAc in Hexane]
  6. customto give a yellow coloured oil

出典と根拠

ORDレコード
ord-6c668f6c9e7f4e829153cb521dd36bea
出典データセット
uspto-grants-2013_08
特許番号
US08501946B2

関連ノート

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