1,3-Dichloroacetone → 2-Acetamido-4-chloromethylthiazole

HRID 272738

反応式

HRID 272738 の反応式
[C:1]([NH:4][C:5]([NH2:7])=[S:6])(=[O:3])[CH3:2].[Cl:8][CH2:9][C:10]([CH2:12]Cl)=O>CC(C)=O.C(OCC)(=O)C>[Cl:8][CH2:9][C:10]1[N:7]=[C:5]([NH:4][C:1](=[O:3])[CH3:2])[S:6][CH:12]=1

参加物

5

反応物 2

HCID 107931,3-DichloroacetoneHCID 2723593Acetylthiourea

生成物 1

HCID 819632-Acetamido-4-chloromethylthiazole

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of acetylthiourea (591 mg, 5 mmol) and 1,3-dichloroacetone (667 mg, 5.25 mmol) in acetone (15 mL) was heated at reflux for 7 hours, cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by column chromatography to give the title compound. MS (DCI) m/e 191 (M+H)+; 1H NMR (300 MHz, DMSO-d6) 12.21 (s, 1H), 7.22 (s, 1H), 4.70 (s, 2H), 2.13 (s, 3H).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 7 hours
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was purified by column chromatography

出典と根拠

ORDレコード
ord-ad2bf5bf99c34722b2d7b275df5bf4b6
出典データセット
uspto-grants-2008_11
特許番号
US07456169B2

関連ノート

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