Sodium Carbonate → Ethyl 1-[2-bis(4-fluorophenyl)methoxyethyl]-4-piperidinecarboxylate

HRID 487141

反応式

HRID 487141 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[O:9][CH2:10][CH2:11]Cl)=[CH:4][CH:3]=1.[NH:20]1[CH2:30][CH2:29][CH:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:22][CH2:21]1.C(=O)([O-])[O-].[Na+].[Na+]>[I-].[K+].C(C(C)=O)C(C)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[O:9][CH2:10][CH2:11][N:20]2[CH2:30][CH2:29][CH:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:22][CH2:21]2)=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 70770Ethyl 4-piperidinecarboxylateHCID 107793021-[Bis(4-fluorophenyl)methoxy]-2-chloroethane

生成物 1

HCID 10069740Ethyl 1-[2-bis(4-fluorophenyl)methoxyethyl]-4-piperidinecarboxylate収率 71.1%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

1.43 g of 1-bis(4-fluorophenyl)methoxy-2-chloroethane and 1.00 g of ethyl isonipecotate were added to 10 ml of methyl isobutyl ketone, and the reaction mixture was then heated under reflux for 5 hours together with 2.0 g of sodium carbonate and 10 mg of potassium iodide. At the end of this time, the mixture was filtered and the solvent was removed by distillation under reduced pressure. The resulting residue was purified by silica gel column chromatography. Elution with a 3:1 by volume mixture of hexane and ethyl acetate afforded 1.45 g (yield 71%) of the title compound as an oily substance.

後処理

  1. temperaturethe reaction mixture was then heated
  2. filtrationAt the end of this time, the mixture was filtered
  3. customthe solvent was removed by distillation under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography
  5. washElution with a 3:1
  6. additionby volume mixture of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-2ba6eac6083142daa3daa7b78ecf6525
出典データセット
uspto-grants-1994_03
特許番号
US05294623

関連ノート

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