Sodium Bicarbonate → HCID 18950739、化合物

HRID 1492558ノート

反応式

HRID 1492558 の反応式
O=[C:2]([C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)[CH2:3][CH2:4][C:5]1[CH:17]=[CH:16][C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:6]=1.[CH:24]([O-:26])=O.[NH4+:27].C(=O)([O-])O.[Na+]>>[CH:24]([NH:27][CH:2]([C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)[CH2:3][CH2:4][C:5]1[CH:17]=[CH:16][C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:6]=1)=[O:26]

参加物

4

反応物 3

HCID 516892Sodium BicarbonateHCID 2723923Ammonium formateHCID 18950751HCID 18950751、化合物

生成物 1

HCID 18950739HCID 18950739、化合物収率 44.6%

実験手順

1.95 g of ethyl 4-[3-oxo-3-(3-pyridyl)propyl]phenoxyacetate and 5.00 g of ammonium formate were stirred at 165° C. for 1.5 hours. To the reaction mixture was added aqueous sodium hydrogencarbonate solution, which was then extracted with ethyl acetate, and the organic phases combined were washed in saturated aqueous sodium chloride, dried over magnesium sulfate, and the solvent was then distilled off. The obtained residue was subjected to chromatography on a silica gel column, and from a fraction eluted with methanol-methylene chloride (5:95 v/v) was obtained 0.95 g of ethyl 4-[3-formamido-3-(3-pyridyl)propyl]phenoxyacetate.

後処理

  1. extractionwas then extracted with ethyl acetate
  2. washthe organic phases combined were washed in saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. distillationthe solvent was then distilled off
  5. washfrom a fraction eluted with methanol-methylene chloride (5:95 v/v)

出典と根拠

ORDレコード
ord-45926debfc114aad9e2bf1f6bc11cb82
出典データセット
uspto-grants-1994_12
特許番号
US05374641

反応ノート

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