6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin → 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin

HRID 1756038笔记

反应方程式

HRID 1756038 反应方程式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH:7][C:8]1[CH:40]=[CH:39][C:11]2[O:12][C:13]([C:16]([N:18]3[CH2:23][CH2:22][N:21]([CH:24]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=4)[C:25]4[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=4)[CH2:20][CH2:19]3)=O)=[CH:14][O:15][C:10]=2[CH:9]=1>C(OCC)C>[OH:7][C:8]1[CH:40]=[CH:39][C:11]2[O:12][C:13]([CH2:16][N:18]3[CH2:19][CH2:20][N:21]([CH:24]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=4)[C:25]4[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=4)[CH2:22][CH2:23]3)=[CH:14][O:15][C:10]=2[CH:9]=1

参与物

4

反应物 2

HCID 98044716-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxinHCID 21226445Aluminium lithium hydride

产物 1

HCID 104338936-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin收率 85%

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

实验过程

Under a nitrogen atmosphere, heat at reflux for 3 hours, in the presence of 5 mmol of lithium aluminium hydride, a solution of 2 mmol of 6-hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin in 35 cm3 of diethyl ether. After cooling, hydrolysis, removal of the insoluble mineral compounds by filtration and drying over magnesium sulfate, the compound obtained is purified by chromatography on a column of silica (eluant: petroleum ether/ethyl acetate, 40:60). 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin is thereby obtained in a yield of 85%. Melting point: 190° C. ##STR79##

后处理

  1. temperatureUnder a nitrogen atmosphere, heat
  2. temperatureAfter cooling
  3. customhydrolysis, removal of the insoluble mineral compounds
  4. filtrationby filtration
  5. dry with materialdrying over magnesium sulfate
  6. customthe compound obtained
  7. customis purified by chromatography on a column of silica (eluant: petroleum ether/ethyl acetate, 40:60)

来源与证据

ORD记录
ord-7ed4eb78a0524eab842045f9adfce8f8
来源数据集
uspto-grants-1995_08
专利号
US05439909

反应笔记

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