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

HRID 1480423노트

반응식

HRID 1480423 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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;

후처리

  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

출처 및 근거

ORD 기록
ord-58e4a99a42c84cf8bbae0b975b869a2c
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409895B2

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