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

HRID 909361ノート

反応式

HRID 909361 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl.[Br:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([NH:26][CH2:27][C:28]([OH:31])([CH3:30])[CH3:29])=[C:14]([NH:19][C:20](=O)[CH2:21][O:22][CH2:23][CH3:24])[CH:15]=[N:16]2)=[N:11][CH:10]=1>C(O)C>[Br:8][C:9]1[CH:10]=[N:11][C:12]2[C:13]3[N:26]([CH2:27][C:28]([CH3:30])([OH:31])[CH3:29])[C:20]([CH2:21][O:22][CH2:23][CH3:24])=[N:19][C:14]=3[CH:15]=[N:16][C:17]=2[CH:18]=1

参加物

4

反応物 2

HCID 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) 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 washed with 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.

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 washed with 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-135db7dfb4414fdd9349cfe2a0f664cc
出典データセット
uspto-grants-2011_09
特許番号
US08017779B2

反応ノート

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