Bromoacetone → HCID 86713417、化合物

HRID 64409

反応式

HRID 64409 の反応式
[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

参加物

5

反応物 3

HCID 11715Bromoacetone2 回HCID 516892Sodium BicarbonateHCID 86713416Methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate

生成物 1

HCID 86713417HCID 86713417、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2d92678427e44e14afb990b87d1e5427
出典データセット
uspto-grants-2016_09
特許番号
US09447090B2

関連ノート

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