Trifluoroacetic acid → 3,3-Dimethylpiperidin-4-one
반응식
C(OC([N:8]1[CH2:13][CH2:12][C:11](=[O:14])[C:10]([CH3:16])([CH3:15])[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:15][C:10]1([CH3:16])[C:11](=[O:14])[CH2:12][CH2:13][NH:8][CH2:9]1참가 물질
4
실험 절차
The 3,3-dimethyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester thus prepared (450 mg, 1.97 mmol) was dissolved in methylene chloride (10 mL). Trifluoroacetic acid was added (305 uL) and the resulting solution stirred at room temperature 2 h. Additional trifluoroacetic acid was added (300 uL) and the reaction stirred at room temperature 3 days. The pale yellow solution was concentrated to afford an oily residue, which was triturated with ether. The solids were collected by suction filtration and dried in vacuo. 3,3-Dimethyl-piperidin-4-one was isolated and used as its trifluoroacetic acid salt (381 mg, 80%).
후처리
- stirringthe reaction stirred at room temperature 3 days
- concentrationThe pale yellow solution was concentrated
- customto afford an oily residue, which
- customwas triturated with ether
- filtrationThe solids were collected by suction filtration
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-56dffb8badf046c4b6812a170c7583af
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07727985B2
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