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Acetic Acid → HCID 21452699, 화합물

HRID 436505
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HRID 436505 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([C:10](=[O:17])[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)N)=[CH:4][CH:3]=1.[C:18]([OH:21])(=[O:20])[CH3:19]>C1CCCCC1>[C:10]([N:8]1[C:3]2[CH2:4][CH:19]([C:18]([OH:21])=[O:20])[CH2:6][CH2:7][C:2]=2[C:6]2[C:5]1=[CH:4][CH:3]=[C:2]([Cl:1])[CH:7]=2)(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 54089464HCID 54089464, 화합물

생성물 1

HCID 21452699HCID 21452699, 화합물

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

A stirred mixture of 2.0 g. of N1 -p-chlorophenyl-N1 -benzoylhydrazine, 1.1 g. of cyclohexanone-3-carboxylic acid, 5 ml. of glacial acetic acid and 7 ml. of cyclohexane were heated under an atmosphere of nitrogen. After 3 hours of stirring at reflux, the reaction mixture was concentrated under reduced pressure and 10 ml. of ethanol was added to the residue. After standing overnight in the refrigerator, the insoluble portion was removed by filtration, washed with a small amount of cold ethanol and dried, yielding 0.4 g. of product, m.p. 196°-197° . Following a recrystallization from ethanol, 0.2 g. of 9-benzoyl-6-chloro-1,2,3,4-tetrahydrocarbazole-2-carboxylic acid was obtained, m.p. 207°-208°.

후처리

  1. additionA stirred mixture of 2.0 g
  2. temperatureat reflux
  3. concentrationthe reaction mixture was concentrated under reduced pressure and 10 ml
  4. additionof ethanol was added to the residue
  5. waitAfter standing overnight in the refrigerator
  6. customthe insoluble portion was removed by filtration
  7. washwashed with a small amount of cold ethanol
  8. customdried
  9. customyielding 0.4 g
  10. customa recrystallization from ethanol, 0.2 g

출처 및 근거

ORD 기록
ord-bf21a542862e41bf9c4c76af71e6088a
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04009181

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