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

HRID 909361노트

반응식

HRID 909361 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
77 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-135db7dfb4414fdd9349cfe2a0f664cc
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017779B2

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