Methyl vinyl ketone → 1-[2-(Bis-(4-fluorophenyl)-methoxy)-ethyl]-4-(3-ketobutyl)piperazine

HRID 1197514노트

반응식

HRID 1197514 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[CH3:25][C:26]([CH:28]=[CH2:29])=[O:27].C(O)(=O)/C=C\C(O)=O>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:18]2[CH:19]=[CH:20][C:21]([F:24])=[CH:22][CH:23]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][N:15]([CH2:29][CH2:28][C:26](=[O:27])[CH3:25])[CH2:14][CH2:13]2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6570Methyl vinyl ketoneHCID 444266Maleic AcidHCID 99740131-[2-[Bis(4-fluorophenyl)methoxy]ethyl]piperazine

생성물 1

HCID 191067251-[2-(Bis-(4-fluorophenyl)-methoxy)-ethyl]-4-(3-ketobutyl)piperazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 0.7 g (2.1 mM) of 1-[2-(bis-(4-fluorophenyl) -methoxy)-ethyl]piperazine and 150 mg (2.1 mM) of freshly distilled methylvinyl-ketone was stirred at room temperature for 2 h. 30 ml of ethanol and 0.48 g of maleic acid were added, the precipitated salt was isolated by filtration and recrystallized from hot acetonitrile to yield the dimaleate salt of the title compound as colourless crystals melting at 159°-160° C. Analytical data were in accordance with the proposed structure.

후처리

  1. customthe precipitated salt was isolated by filtration
  2. customrecrystallized from hot acetonitrile

출처 및 근거

ORD 기록
ord-aa1d00423dba468ebc12f1be8a6b059b
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05276035

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