Acetic Acid → HCID 68138826, 화합물

HRID 1578692노트

반응식

HRID 1578692 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 68138826HCID 68138826, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7028a80601274b37b4bdf27c413e94b1
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03939159

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