Acetic Acid → HCID 68138826、化合物

HRID 1578692ノート

反応式

HRID 1578692 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.C(O)(=O)C.[NH2:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1[N:21]1[CH:25]=[CH:24][CH:23]=[CH:22]1>C(O)C>[ClH:20].[Cl:20][C:18]1[CH:19]=[C:14]2[C:15](=[CH:16][CH:17]=1)[N:21]1[CH:22]=[CH:23][CH:24]=[C:25]1[C:5]1([CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)[NH:13]2

参加物

5

反応物 3

HCID 176Acetic AcidHCID 740491-Methyl-4-piperidoneHCID 106554015-chloro-2-(1H-pyrrol-1-yl)aniline

生成物 1

HCID 68138826HCID 68138826、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1.7 g (0.016 mole) of 1-methyl-4-piperidone and 3 ml. of glacial acetic acid are added to a solution of 2.7 g (0.014 mole) of 1-(2-amino-4-chloro-phenyl) pyrrole, Example 13(b), in 50 ml. of absolute ethanol. The solution is refluxed for 36 hours and concentrated, and the residue dissolved in water. The aqueous solution is filtered, and the filtrate is basified. A solid precipitates, is filtered, and dried. The solid is dissolved in ether and ethereal-hydrogen chloride is added. The resulting precipitate is filtered, dried, and recrystallized from methanol to give 7-chloro-4,5-dihydro-1'-methylspiro-[pyrrolo (1,2-a)quinoxaline-4,4'-piperidine] hydrochloride, m.p. 297°-298° C.

後処理

  1. temperatureThe solution is refluxed for 36 hours
  2. concentrationconcentrated
  3. dissolutionthe residue dissolved in water
  4. filtrationThe aqueous solution is filtered
  5. customA solid precipitates
  6. filtrationis filtered
  7. customdried
  8. dissolutionThe solid is dissolved in ether
  9. additionethereal-hydrogen chloride is added
  10. filtrationThe resulting precipitate is filtered
  11. customdried
  12. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-7028a80601274b37b4bdf27c413e94b1
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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