Sodium Bicarbonate → 6-[3-(tert-Butyldimethylsilanyloxymethyl)phenyl]-2-(2,4-difluorophenyl)-3-methylimidazo[1,2-a]pyridine

HRID 1891238

反応式

HRID 1891238 の反応式
[Si:1]([O:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[CH:17]=[CH:18][C:19]([NH2:22])=[N:20][CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(=O)([O-])O.[Na+].Br[CH:29]([CH3:40])[C:30]([C:32]1[CH:37]=[CH:36][C:35]([F:38])=[CH:34][C:33]=1[F:39])=O>C(O)C>[Si:1]([O:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[CH:17]=[CH:18][C:19]3[N:20]([C:29]([CH3:40])=[C:30]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][C:33]=4[F:39])[N:22]=3)[CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 110758302-Bromo-1-(2,4-difluorophenyl)propan-1-oneHCID 44232378HCID 44232378、化合物

生成物 1

HCID 698104776-[3-(tert-Butyldimethylsilanyloxymethyl)phenyl]-2-(2,4-difluorophenyl)-3-methylimidazo[1,2-a]pyridine収率 49.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

300 mg of 5-[3-(tert-butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine dissolved in 5 ml of ethanol are placed in a screw reactor. 200 mg of sodium hydrogen carbonate and 470 mg of 2-bromo-1-(2,4-difluorophenyl)propan-1-one are added thereto. The reactor is closed and heated at 80° C. for 20 h. After cooling, the reaction mixture is concentrated under reduced pressure. The residue obtained is purified by silica gel chromatography, elution being carried out with a heptane/ethyl acetate mixture. 220 mg of compound are obtained.

後処理

  1. customare placed in a screw reactor
  2. customThe reactor is closed
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated under reduced pressure
  5. customThe residue obtained
  6. customis purified by silica gel chromatography, elution

出典と根拠

ORDレコード
ord-4fec0477d0454ff7882f382327028793
出典データセット
uspto-grants-2013_08
特許番号
US08507520B2

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