Water → 2-(4-Fluorobenzoyl)-3-propoxypyridine

HRID 856639노트

반응식

HRID 856639 반응식
C([CH:3]([C:11]1[C:16]([O:17][CH2:18][CH2:19][CH3:20])=[CH:15][CH:14]=[CH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][CH:5]=1)#N.C(=O)([O-])[O-:22].[K+].[K+].O>CS(C)=O.O>[F:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([C:11]2[C:16]([O:17][CH2:18][CH2:19][CH3:20])=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:22])=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 229387622-(alpha-Cyano-4-fluorobenzyl)-3-propoxypyridine

생성물 1

HCID 229388512-(4-Fluorobenzoyl)-3-propoxypyridine수율 85.8%

시약·촉매·용매 1

HCID 23503278(Methanesulfinyl)methane--water (1/1)용매

실험 절차

Under oxygen atmosphere, a mixed solution of 2-(α-cyano-4-fluorobenzyl)-3-propoxypyridine (5.42 g) and potassium carbonate (3.07 g) in DMSO-water (200-40 ml) was stirred at room temperature for 20 hours. The reaction mixture was added to water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and concentrated under reduced pressure, and the obtained residue was separated and purified by column chromatography (ethyl acetate:hexane 1:3→1:2), to give 2-(4-fluorobenzoyl)-3-propoxypyridine (4.46 g) as pale yellow oil.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customthe obtained residue was separated
  6. custompurified by column chromatography (ethyl acetate:hexane 1:3→1:2)

출처 및 근거

ORD 기록
ord-793936c7b05241bdac86b1b253dfbee6
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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