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

HRID 272738

반응식

HRID 272738 반응식
[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

참가 물질

5

반응물 2

HCID 107931,3-DichloroacetoneHCID 2723593Acetylthiourea

생성물 1

HCID 819632-Acetamido-4-chloromethylthiazole

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ad2bf5bf99c34722b2d7b275df5bf4b6
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456169B2

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