Hydrochloric Acid → 6-Azaindole
反応式
C(OC([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[N:14][CH:15]=2)[CH2:10][CH:9]1O)=O)(C)(C)C.Cl.[OH-].[Na+]>O1CCCC1>[NH:8]1[C:16]2=[CH:15][N:14]=[CH:13][CH:12]=[C:11]2[CH:10]=[CH:9]1参加物
5
反応条件
- 温度
- 50 °C
実験手順
The azaindoline (step b, 1.1 g, 5.0 mmol) was dissolved in tetrahydrofuran (20 ml) and treated with 5.5M hydrochloric acid (5 ml). The mixture was heated at 50° C. for 4.5 hours cooled to 0° C. and basified with 5M sodium hydroxide (7.0 ml). The mixture was extracted with ethyl acetate (2×20 ml) and the combined ethyl acetate fractions were washed with saturated brine (20 ml), dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound as a pale yellow crystalline solid; yield: 0.57 g (97%). mp. 132°-134° C.[Lit. mp 131°-132° C.].
後処理
- temperaturecooled to 0° C.
- extractionThe mixture was extracted with ethyl acetate (2×20 ml)
- washthe combined ethyl acetate fractions were washed with saturated brine (20 ml)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-0652b9c08d2d4c839124c5d6edbaa19a
- 出典データセット
- uspto-grants-1997_10
- 特許番号
- US05681959
反応ノート
読み込み中…