Trifluoroacetic acid → Methyl 3-(3-aminopiperidin-1-yl)benzoate

HRID 602161노트

반응식

HRID 602161 반응식
FC(F)(F)C(O)=O.C(OC([NH:15][CH:16]1[CH2:21][CH2:20][CH2:19][N:18]([C:22]2[CH:23]=[C:24]([CH:29]=[CH:30][CH:31]=2)[C:25]([O:27][CH3:28])=[O:26])[CH2:17]1)=O)(C)(C)C>ClCCl>[NH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][N:18]([C:22]2[CH:23]=[C:24]([CH:29]=[CH:30][CH:31]=2)[C:25]([O:27][CH3:28])=[O:26])[CH2:17]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 58992690Methyl 3-[3-(tert-butoxycarbonylamino)piperidin-1-yl]benzoate

생성물 1

HCID 58992611Methyl 3-(3-aminopiperidin-1-yl)benzoate수율 50%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (2 mL) was added to methyl 3-[3-(tert-butoxycarbonylamino)piperidin-1-yl]benzoate (451 mg, 1.35 mmol) in dichloromethane (2 mL). The reaction mixture was stirred at room temperature for 1 hour. Subsequently, the mixture was concentrated and a saturated aqueous sodium bicarbonate solution was added to the residue to make it basic. The mixture was extracted with ethyl acetate and the organic layer washed with brine and dried over magnesium sulfate. Evaporation of the solvent gave 158 mg (50%) of the desired compound as a pale yellow oil.

후처리

  1. concentrationSubsequently, the mixture was concentrated
  2. additiona saturated aqueous sodium bicarbonate solution was added to the residue
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic layer washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-9e2848ca960545a1bf7b7cc77d96c5f3
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902367B2

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