Trifluoroacetic acid → (E)-1-(4-(2-Aminoethyl)piperidin-1-yl)-3-(3,5-dichlorophenyl)prop-2-en-1-one

HRID 1480423ノート

反応式

HRID 1480423 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16](=[O:27])/[CH:17]=[CH:18]/[C:19]2[CH:24]=[C:23]([Cl:25])[CH:22]=[C:21]([Cl:26])[CH:20]=2)[CH2:12][CH2:11]1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:7][CH2:8][CH2:9][CH:10]1[CH2:11][CH2:12][N:13]([C:16](=[O:27])/[CH:17]=[CH:18]/[C:19]2[CH:24]=[C:23]([Cl:25])[CH:22]=[C:21]([Cl:26])[CH:20]=2)[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86722653(E)-tert-Butyl (2-(1-(3-(3,5-dichlorophenyl)acryloyl)piperidin-4-yl)ethyl)carbamate

生成物 1

HCID 86722654(E)-1-(4-(2-Aminoethyl)piperidin-1-yl)-3-(3,5-dichlorophenyl)prop-2-en-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To (E)-tert-butyl(2-(1-(3-(3,5-dichlorophenyl)acryloyl)piperidin-4-yl)ethyl)carbamate (step 3) (400 mg, 0.936 mmol) in DCM (5 ml) was added TFA (0.865 ml, 11.23 mmol) and the mixture was stirred at RT for 1 h. The solvent was removed under reduced pressure and the crude material was dissolved in MeOH and loaded on to an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with excess MeOH. The product was eluted using 2.0 M ammonia in MeOH and the solvent removed under reduced pressure to afford the title compound as a white solid;

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe crude material was dissolved in MeOH
  3. washThe cartridge was washed with excess MeOH
  4. washThe product was eluted
  5. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-58e4a99a42c84cf8bbae0b975b869a2c
出典データセット
uspto-grants-2016_08
特許番号
US09409895B2

反応ノート

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