Sodium Bicarbonate → HCID 18950739, 화합물

HRID 1492558노트

반응식

HRID 1492558 반응식
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]

참가 물질

4

반응물 3

HCID 516892Sodium BicarbonateHCID 2723923Ammonium formateHCID 18950751HCID 18950751, 화합물

생성물 1

HCID 18950739HCID 18950739, 화합물수율 44.6%

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-45926debfc114aad9e2bf1f6bc11cb82
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05374641

반응 노트

불러오는 중…