Sodium Methoxide → 8-(Methoxy)-2-{[2-(methyloxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-2-yl)-9H-Purin-6-amine
반응식
Br[C:2]1[N:3]([CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][O:18]2)[C:4]2[C:9]([N:10]=1)=[C:8]([NH2:11])[N:7]=[C:6]([O:12][CH2:13][CH2:14][O:15][CH3:16])[N:5]=2.[CH3:23][O-:24].[Na+]>CO>[CH3:23][O:24][C:2]1[N:3]([CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][O:18]2)[C:4]2[C:9]([N:10]=1)=[C:8]([NH2:11])[N:7]=[C:6]([O:12][CH2:13][CH2:14][O:15][CH3:16])[N:5]=2참가 물질
반응 조건
- 온도
- 65 °C
실험 절차
8-Bromo-2-{[2-(methoxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (1.4489 g) was suspended in dry methanol (11.5 mL) and then treated with 25% (w/v) sodium methoxide in methanol (2.5 mL). The reaction mixture was heated to reflux (65° C., externally) were upon a solution was obtained. After 4 hours the reaction mixture was concentrated under reduced pressure and saturated aqueous ammonium chloride (100 mL) was added. This was then extracted with ethyl acetate (100 mL, twice). The organic layers was separated, combined and washed with brine (100 mL). The organic layer was separated and then dried by passing through a hydrophobic frit. This was then evaporated under reduced pressure to give the title compound as a white solid (1.2032 g) after placing under high vacuo, overnight.
후처리
- temperatureThe reaction mixture was heated
- customwas obtained
- concentrationAfter 4 hours the reaction mixture was concentrated under reduced pressure and saturated aqueous ammonium chloride (100 mL)
- additionwas added
- extractionThis was then extracted with ethyl acetate (100 mL
- customThe organic layers was separated
- washwashed with brine (100 mL)
- customThe organic layer was separated
- customdried
- customThis was then evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-e8f772580f5c45a2b5409042f4f9f7d5
- 출처 데이터셋
- uspto-grants-2011_07
- 특허 번호
- US07977344B2
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