Trifluoroacetic acid → HCID 3773118, 화합물
반응식
[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]참가 물질
6
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f70a40aeaed443b68081e7b32c6f617e
- 출처 데이터셋
- uspto-grants-1998_07
- 특허 번호
- US05776983
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