Trifluoroacetic acid → 1-Amino-6-(4-fluorophenyl)piperidin-2-one

HRID 1803216ノート

反応式

HRID 1803216 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][CH2:11][C:10](=[O:14])[N:9]2[NH:15]C(=O)OC(C)(C)C)=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl.CCOC(C)=O>[NH2:15][N:9]1[CH:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[CH2:13][CH2:12][CH2:11][C:10]1=[O:14]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 66859411Tert-butyl 2-(4-fluorophenyl)-6-oxopiperidin-1-ylcarbamate

生成物 1

HCID 581101281-Amino-6-(4-fluorophenyl)piperidin-2-one収率 90%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Step AAG (3): To a soln of tert-butyl 2-(4-fluorophenyl)-6-oxopiperidin-1-ylcarbamate (330 mg, 1.07 mmol) in CH2Cl2 (5 mL) was added TFA (1.00 mL, 13.0 mmol). The mixture was stirred at for 2 hrs. The solvent was removed in vacuo. The crude reaction was diluted with EtOAc (100 mL). The organic layer was separated and washed with saturated aqueous NaHCO3 solution, dried over Na2SO4, filtered, and concentrated in vacuo to afford 1-amino-6-(4-fluorophenyl)piperidin-2-one (200 mg, 90% yield). LC-MS (M+H)+ 209.26.

後処理

  1. customThe solvent was removed in vacuo
  2. customThe crude reaction
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous NaHCO3 solution
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f701bac0489543e08125eb6b6730117d
出典データセット
uspto-grants-2013_01
特許番号
US08349880B2

反応ノート

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