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Acetic Acid → HCID 21452699、化合物

HRID 436505
ノート
印刷プレビュー

反応式

HRID 436505 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 176Acetic AcidHCID 54089464HCID 54089464、化合物

生成物 1

HCID 21452699HCID 21452699、化合物

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-bf21a542862e41bf9c4c76af71e6088a
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04009181

反応ノート

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