Trifluoroacetic acid → 3,3-Dimethylpiperidin-4-one

HRID 12250

반응식

HRID 12250 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]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 22278899tert-Butyl 3,3-dimethyl-4-oxopiperidine-1-carboxylate

생성물 1

HCID 222788373,3-Dimethylpiperidin-4-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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

  1. stirringthe reaction stirred at room temperature 3 days
  2. concentrationThe pale yellow solution was concentrated
  3. customto afford an oily residue, which
  4. customwas triturated with ether
  5. filtrationThe solids were collected by suction filtration
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-56dffb8badf046c4b6812a170c7583af
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727985B2

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