Trifluoroacetic acid → N-Methyl-N-(piperidin-4-yl)benzamide

HRID 2168193노트

반응식

HRID 2168193 반응식
[CH3:1][N:2]([C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:17])[CH:3]1[CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][CH2:4]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][N:2]([CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)[C:16](=[O:17])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67977238HCID 67977238, 화합물

생성물 1

HCID 12641853N-Methyl-N-(piperidin-4-yl)benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1-dimethylethyl 4-[methyl(phenylcarbonyl)amino]-1-piperidinecarboxylate D14 (1.66 g) was dissolved in DCM (5 mL) then TFA (4.02 mL, 52.1 mmol) was slowly added. The reaction was stirred at room temperature for 30 minutes. TFA and DCM were removed in vacuo. The crude mixture was poured on a top of an Isolute Si—SCX-2 cartridge, eluting with DCM then MeOH then a 2M NH3 in MeOH solution. Fractions containing desired compound were evaporated in vacuo to give title compound D15 in 1.18 g. LCMS [M+H][email protected] min (2 min run)

후처리

  1. customTFA and DCM were removed in vacuo
  2. additionThe crude mixture was poured on a top of an Isolute Si—SCX-2 cartridge
  3. washeluting with DCM
  4. additionFractions containing desired compound
  5. customwere evaporated in vacuo

출처 및 근거

ORD 기록
ord-fa1f97b294e3473f8c26d1eaebe79171
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09045485B2

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