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

HRID 1891238

반응식

HRID 1891238 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4fec0477d0454ff7882f382327028793
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507520B2

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