Sodium ethoxide → 7-(4-Amino-3-fluorophenoxy)-1-N-methyl-1H-imidazo[4,5-b]pyridin-2(3H)-one

HRID 2409257노트

반응식

HRID 2409257 반응식
[NH2:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([NH2:13])[C:8]=2[N:14]([CH3:20])[C:15](=O)[O:16]CC)=[CH:4][C:3]=1[F:23].CC[O-].[Na+].[Na]>CCO>[NH2:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]3[NH:13][C:15](=[O:16])[N:14]([CH3:20])[C:8]=23)=[CH:4][C:3]=1[F:23]

참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 44184953Ethyl 4-(4-amino-3-fluorophenoxy)-2-aminopyridin-3-yl-methyl-carbamate

생성물 1

HCID 441849547-(4-Amino-3-fluorophenoxy)-1-N-methyl-1H-imidazo[4,5-b]pyridin-2(3H)-one

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
100 °C

실험 절차

Ethyl 4-(4-amino-3-fluorophenoxy)-2-aminopyridin-3-yl-methyl-carbamate (7a) (320 mg, 1.0 mmol) was suspended in a solution of EtONa in EtOH (4 mL), obtained from dissolving sodium (480 mg, 21 mmol) in ethanol (9 mL). The suspension was heated under microwave irradiation for 1 hour (100° C., 100 W). The mixture was cooled at room temperature and the solvent was evaporated. The residue was dissolved in water and was acidified with AcOH to pH 4. The precipitate formed was recovered by filtration, to afford the title compound.

후처리

  1. customobtained
  2. temperatureThe mixture was cooled at room temperature
  3. customthe solvent was evaporated
  4. dissolutionThe residue was dissolved in water
  5. customThe precipitate formed
  6. filtrationwas recovered by filtration

출처 및 근거

ORD 기록
ord-308f0562f41c4810986ef820fb50e176
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815896B2

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