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

HRID 2168193ノート

反応式

HRID 2168193 の反応式
[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

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67977238HCID 67977238、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-fa1f97b294e3473f8c26d1eaebe79171
出典データセット
uspto-grants-2015_06
特許番号
US09045485B2

反応ノート

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