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

HRID 1197514ノート

反応式

HRID 1197514 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-aa1d00423dba468ebc12f1be8a6b059b
出典データセット
uspto-grants-1994_01
特許番号
US05276035

反応ノート

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