Trifluoroacetic acid → 1-{1-[4-(Trifluoromethyl)phenyl]piperidin-4-yl}methanamine

HRID 2093586노트

반응식

HRID 2093586 반응식
FC(F)(F)C(O)=O.C(OC(=O)[NH:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=2)[CH2:18][CH2:17]1)(C)(C)C>ClCCl>[F:30][C:28]([F:29])([F:31])[C:25]1[CH:24]=[CH:23][C:22]([N:19]2[CH2:20][CH2:21][CH:16]([CH2:15][NH2:14])[CH2:17][CH2:18]2)=[CH:27][CH:26]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66853254Tert-butyl({1-[4-(trifluoromethyl)phenyl]piperidin-4-yl}methyl)carbamate

생성물 1

HCID 595860101-{1-[4-(Trifluoromethyl)phenyl]piperidin-4-yl}methanamine수율 123.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of trifluoroacetic acid (10 ml) and dichloromethane (10 ml) was added to tert-butyl({1-[4-(trifluoromethyl)phenyl]piperidin-4-yl}methyl)carbamate (1.36 g). This mixture was stirred at room temperature for 3 h. The sample was concentrated and taken up in dichloromethane (20 ml) and saturated aqueous sodium bicarbonate. The mixture was extracted and the organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to provide the title compound (1.21 g, 86%). Mass spectrum (ESI) 242.1 (M+1).

후처리

  1. concentrationThe sample was concentrated
  2. extractionThe mixture was extracted
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-071f88bfa2834bc49a00051e172efd00
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445480B2

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