1,3-Dichloroacetone → 4-(Chloromethyl)-2-(propan-2-yl)-1,3-thiazole--hydrogen chloride (1/1)

HRID 52689

反応式

HRID 52689 の反応式
[CH3:1][CH:2]([CH3:6])[C:3](=[S:5])[NH2:4].[Cl:7][CH2:8][C:9]([CH2:11]Cl)=O.[O-]S([O-])(=O)=O.[Mg+2]>CC(C)=O>[ClH:7].[Cl:7][CH2:8][C:9]1[N:4]=[C:3]([CH:2]([CH3:6])[CH3:1])[S:5][CH:11]=1

参加物

5

反応物 3

HCID 107931,3-DichloroacetoneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 109095072-Methylpropanethioamide

生成物 1

HCID 187588464-(Chloromethyl)-2-(propan-2-yl)-1,3-thiazole--hydrogen chloride (1/1)

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3.5 h
  3. temperatureto cool
  4. filtrationfiltered
  5. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-a7eb556908204482bceb93a605ec7ad7
出典データセット
uspto-grants-1997_04
特許番号
US05616720

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