Bromoacetone → HCID 86713417, 화합물

HRID 64409

반응식

HRID 64409 반응식
[NH2:1][C:2]1[C:11]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[F:20])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=1.Br[CH2:22][C:23](=O)[CH3:24].C(=O)([O-])O.[Na+]>C(O)C>[F:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][O:12][C:11]1[C:2]2[N:3]([CH:22]=[C:23]([CH3:24])[N:1]=2)[CH:4]=[C:5]([C:6]([O:8][CH3:9])=[O:7])[CH:10]=1

참가 물질

5

반응물 3

HCID 11715Bromoacetone2회HCID 516892Sodium BicarbonateHCID 86713416Methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate

생성물 1

HCID 86713417HCID 86713417, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To a suspension of 2.15 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate in 43 ml of ethanol was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the solvent was evaporated under reduced pressure, followed by extracting with ethyl acetate and washing with saturated brine. After drying over anhydrous magnesium sulfate and then filtering, the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.39 g of methyl 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylate.

후처리

  1. stirringby stirring at 80° C. for 4 hours
  2. customthe solvent was evaporated under reduced pressure
  3. extractionby extracting with ethyl acetate
  4. washwashing with saturated brine
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. filtrationfiltering
  7. customthe solvent was evaporated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2d92678427e44e14afb990b87d1e5427
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447090B2

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