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3-Chloro-2,4-pentanedione → HCID 9344223, 화합물

HRID 1498946
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HRID 1498946 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[S:5].Cl[CH:13]([C:17](=O)[CH3:18])[C:14](=[O:16])[CH3:15]>C(O)C>[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]1[S:5][C:13]([C:14](=[O:16])[CH3:15])=[C:17]([CH3:18])[N:6]=1
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참가 물질

4

반응물 2

HCID 743283-Chloro-2,4-pentanedioneHCID 25176802,4-Dimethylbenzenecarbothioamide

생성물 1

HCID 9344223HCID 9344223, 화합물수율 37%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To ethanol (20 ml), 2,4-dimethylthiobenzamide (2.00 g) and 3-chloropentane-2,4-dione (1.79 g) were added, and the mixture was stirred under heat reflux for 4 hours. After the mixture was allowed to cool to a room temperature, from the mixture ethanol was distilled off under a reduced pressure. To the resulting residue, ethyl acetate was added, and the mixture was heated and stirred. After the mixture was allowed to cool to a room temperature, the precipitate was separated by filtration, washed with ethyl acetate, and then dried under a reduced pressure to give the title compound (1.10 g, 37%).

후처리

  1. temperatureunder heat
  2. temperaturereflux for 4 hours
  3. distillationwas distilled off under a reduced pressure
  4. additionTo the resulting residue, ethyl acetate was added
  5. temperaturethe mixture was heated
  6. stirringstirred
  7. customthe precipitate was separated by filtration
  8. washwashed with ethyl acetate
  9. customdried under a reduced pressure

출처 및 근거

ORD 기록
ord-532f438747f44bc58a01e1341693363c
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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