7-(Dimethoxymethyl)-1,2,3,4-tetrahydro-1,8-naphthyridine → 5,6,7,8-Tetrahydro-1,8-naphthyridine-2-carbaldehyde
反応式
C[O:2][CH:3](OC)[C:4]1[CH:13]=[CH:12][C:11]2[CH2:10][CH2:9][CH2:8][NH:7][C:6]=2[N:5]=1>FC(F)(F)C(O)=O>[N:5]1[C:6]2[NH:7][CH2:8][CH2:9][CH2:10][C:11]=2[CH:12]=[CH:13][C:4]=1[CH:3]=[O:2]参加物
3
実験手順
8-2 (10 g, 0.048 mol) was treated with trifluoroacetic acid (50 mL) and the resulting solution stirred under argon for 12.5 h. The TFA was removed at reduced pressure and the residue partitioned between sat. NaHCO3 and CH2Cl2. The organic layer was dried, concentrated and passed through a 3 in. pad of silica gel (10% acetone/CH2Cl2) and concentrated to afford 8-3 as a yellow crystalline solid.
後処理
- customThe TFA was removed at reduced pressure
- customthe residue partitioned between sat. NaHCO3 and CH2Cl2
- customThe organic layer was dried
- concentrationconcentrated
- concentrationpad of silica gel (10% acetone/CH2Cl2) and concentrated
出典と根拠
- ORDレコード
- ord-81333ece685042648560ab860a57270d
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06297249B1
反応ノート
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