Trifluoroacetic acid → HCID 3773118、化合物
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]([C:16]#[N:17])[C:12]([O:14][CH3:15])=[O:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(O)(C(F)(F)F)=O.[H][H]>[Pd].CO>[NH2:17][CH2:16][CH:11]([C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[C:12]([O:14][CH3:15])=[O:13]参加物
6
実験手順
A MeOH solution (100 mL) containing methyl 3,4-dimethoxyphenylcyanoacetate (1.2 g, 5.1 mmol), TFA (1 mL), and 50 mg of 10% Pd/C was shaken on a Parr shaker for 20 hours under 30 psi of hydrogen. The reaction was filtered, concentrated, dissolved in H2O, and extracted 2× with Et2O. The pH was adjusted to ~10 and the mixture extracted 3× with EtOAc. The EtOAc fractions were dried over Na2SO4 and concentrated to yield 400 mg (32%) of the title compound.
後処理
- filtrationThe reaction was filtered
- concentrationconcentrated
- dissolutiondissolved in H2O
- extractionextracted 2× with Et2O
- extractionthe mixture extracted 3× with EtOAc
- dry with materialThe EtOAc fractions were dried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f70a40aeaed443b68081e7b32c6f617e
- 出典データセット
- uspto-grants-1998_07
- 特許番号
- US05776983
反応ノート
読み込み中…