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

HRID 59035ノート

反応式

HRID 59035 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-23acdab3e7b243d78574d98717d37ab8
出典データセット
uspto-grants-2016_09
特許番号
US09439893B2

反応ノート

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