Acetic Acid → HCID 21558493、化合物

HRID 1578693ノート

反応式

HRID 1578693 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(=O)C.[NH2:19][C:20]1[CH:25]=[C:24]([Cl:26])[CH:23]=[CH:22][C:21]=1[N:27]1[CH:31]=[CH:30][CH:29]=[CH:28]1>C(O)C>[ClH:26].[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]2([NH:19][C:20]3[C:21](=[CH:22][CH:23]=[C:24]([Cl:26])[CH:25]=3)[N:27]3[CH:28]=[CH:29][CH:30]=[C:31]23)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 192201-Benzyl-4-piperidoneHCID 106554015-chloro-2-(1H-pyrrol-1-yl)aniline

生成物 1

HCID 21558493HCID 21558493、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5.29 g (0.028 mole) of 1-benzyl-4-piperidone and 2 ml. of glacial acetic acid are added to a solution of 5.0 g (0.026 mole) of 1-(2-amino-4-chlorophenyl)pyrrole [Example 13(b)] in 80 ml. of absolute ethanol. The solution is refluxed, leaving a yellow oil. The oil is washed with a potassium hydroxide solution, then water, and placed in a refrigerator overnight. The tan solid which forms is dissolved in ether, and ethereal hydrogen chloride is added. The resulting precipitate is washed with water and dried to give 1'-benzyl-7-chloro-4,5-dihydrospiro[pyrrolo(1,2-a)quinoxaline-4,4'-piperidine]hydrochloride, m.p. 282°-283° C.

後処理

  1. temperatureThe solution is refluxed
  2. customleaving a yellow oil
  3. washThe oil is washed with a potassium hydroxide solution
  4. customplaced in a refrigerator overnight
  5. dissolutionThe tan solid which forms is dissolved in ether
  6. additionethereal hydrogen chloride is added
  7. washThe resulting precipitate is washed with water
  8. customdried

出典と根拠

ORDレコード
ord-1634684d88724983a4033613af82b950
出典データセット
uspto-grants-1976_02
特許番号
US03939159

反応ノート

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