Sodium Methoxide → 8-(Methoxy)-2-{[2-(methyloxy)ethyl]oxy}-9-(tetrahydro-2H-pyran-2-yl)-9H-Purin-6-amine
反応式
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]=2参加物
反応条件
- 温度
- 65 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-e8f772580f5c45a2b5409042f4f9f7d5
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07977344B2
反応ノート
読み込み中…