Hydrogen Bromide → HCID 178448441、化合物
反応式
[C:1]([N:5]1[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][N:9]=[C:10]([O:15]C)[CH:11]=2)[CH2:6]1)([CH3:4])([CH3:3])[CH3:2].Br>C(O)(=O)C>[C:1]([N:5]1[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][N:9]=[C:10]([OH:15])[CH:11]=2)[CH2:6]1)([CH3:4])([CH3:2])[CH3:3]参加物
4
実験手順
A solution of 2-tert-butyl-6-methoxy-1,2,3,4-tetrahydro-2,7-naphthyridine (5.1 g, 23 mmol) and 45% hydrobromic acid in acetic acid (70 mL) was heated in a sealed tube at 100° C. for 1 h, cooled to RT and concentrated. The residue was dissolved carefully in 20% potassium carbonate solution (100 mL) and extracted four times with EtOAc. The combined organic phases were dried, filtered and concentrated. Recrystallisation from TBME-hexanes gave 3.7 g (77%) of the title compound as a white solid.
後処理
- concentrationconcentrated
- dissolutionThe residue was dissolved carefully in 20% potassium carbonate solution (100 mL)
- extractionextracted four times with EtOAc
- customThe combined organic phases were dried
- filtrationfiltered
- concentrationconcentrated
- customRecrystallisation from TBME-hexanes
出典と根拠
- ORDレコード
- ord-9e10929e2730498c820abf8dc3040884
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07655664B2
反応ノート
読み込み中…