Water → 1-[7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol

HRID 598014ノート

反応式

HRID 598014 の反応式
C(=O)([O-])[O-].[K+].[K+].O.Cl.[Br:9][C:10]1[CH:19]=[C:18]2[C:13]([C:14]([NH:27][CH2:28][C:29]([OH:32])([CH3:31])[CH3:30])=[C:15]([NH:20][C:21](=O)[CH2:22][O:23][CH2:24][CH3:25])[CH:16]=[N:17]2)=[N:12][CH:11]=1>C(O)C>[Br:9][C:10]1[CH:11]=[N:12][C:13]2[C:14]3[N:27]([CH2:28][C:29]([CH3:31])([OH:32])[CH3:30])[C:21]([CH2:22][O:23][CH2:24][CH3:25])=[N:20][C:15]=3[CH:16]=[N:17][C:18]=2[CH:19]=1

参加物

5

反応物 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 67052474N-{7-bromo-4-[(2-hydroxy-2-methylpropyl)amino][1,5]naphthyridin-3-yl}-2-ethoxyacetamide hydrochloride

生成物 1

HCID 670524691-[7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol収率 90.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
77 °C

実験手順

Potassium carbonate (113 g) and deionized water (565 mL) were sequentially added to a solution of N-{7-bromo-4-[(2-hydroxy-2-methylpropyl)amino][1,5]naphthyridin-3-yl}-2-ethoxyacetamide hydrochloride (113 g, 261 mmol) in denatured ethanol (1.695 L), and the resulting mixture was heated at reflux (77° C.) overnight and allowed to cool to room temperature. The ethanol was removed under reduced pressure, and the resulting mixture was filtered to isolate a solid. The solid was washed with deionized water (100 mL) and dried over two nights in a vacuum oven at 40° C. to provide 90 g of 1-[7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol as a brown solid. Material from a separate run was used in the next step.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureto cool to room temperature
  3. customThe ethanol was removed under reduced pressure
  4. filtrationthe resulting mixture was filtered
  5. customto isolate a solid
  6. washThe solid was washed with deionized water (100 mL)
  7. customdried over two nights in a vacuum oven at 40° C.

出典と根拠

ORDレコード
ord-713d03a22cac4dae8ceb36409ba3dd3d
出典データセット
uspto-grants-2011_03
特許番号
US07897609B2

反応ノート

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