홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Trifluoroacetic acid → N-{[(3S)-3-Fluoro-3-piperidinyl]methyl}-7-{1-[(methyloxy)methyl]-1H-pyrazol-4-yl}-1,6-naphthyridin-5-amine

HRID 473327
노트
인쇄 미리보기

반응식

HRID 473327 반응식
[F:1][C@@:2]1([CH2:15][NH:16][C:17]2[N:26]=[C:25]([C:27]3[CH:28]=[N:29][N:30]([CH2:32][O:33][CH3:34])[CH:31]=3)[CH:24]=[C:23]3[C:18]=2[CH:19]=[CH:20][CH:21]=[N:22]3)[CH2:7][CH2:6][CH2:5][N:4](C(OC(C)(C)C)=O)[CH2:3]1.FC(F)(F)C(O)=O>C(Cl)Cl>[F:1][C@@:2]1([CH2:15][NH:16][C:17]2[C:18]3[CH:19]=[CH:20][CH:21]=[N:22][C:23]=3[CH:24]=[C:25]([C:27]3[CH:28]=[N:29][N:30]([CH2:32][O:33][CH3:34])[CH:31]=3)[N:26]=2)[CH2:7][CH2:6][CH2:5][NH:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 682098891,1-Dimethylethyl (3R)-3-fluoro-3-{[(7-{1-[(methyloxy)methyl]-1H-pyrazol-4-yl}-1,6-naphthyridin-5-yl)amino]methyl}-1-piperidinecarboxylate

생성물 1

HCID 54575461N-{[(3S)-3-Fluoro-3-piperidinyl]methyl}-7-{1-[(methyloxy)methyl]-1H-pyrazol-4-yl}-1,6-naphthyridin-5-amine수율 54.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 1,1-dimethylethyl (3R)-3-fluoro-3-{[(7-{1-[(methyloxy)methyl]-1H-pyrazol-4-yl}-1,6-naphthyridin-5-yl)amino]methyl}-1-piperidinecarboxylate (813 mg, 1.728 mmol) in DCM (10 ml) was added trifluoroacetic acid (2 ml, 26.0 mmol) and stirred at room temperature for 2 h. LCMS showed product as the main peak. The solvent was removed and dissolved in methanol and loaded onto a pre-equilibrated 50 g SCX cartridge. Washed with methanol and eluted with 2M methanolic ammonia. The solvent from the ammonia fractions was removed and the residue dried under high vacuum overnight. The residue was purified on the large scale high pH MDAP (Method D). Appropriate fractions were combined and the solvent removed. The resulting product was dried under high vacuum for 1 h to give the title compound as a yellow solid (349 mg).

후처리

  1. customThe solvent was removed
  2. dissolutiondissolved in methanol
  3. washWashed with methanol
  4. washeluted with 2M methanolic ammonia
  5. customThe solvent from the ammonia fractions was removed
  6. customthe residue dried under high vacuum overnight
  7. customThe residue was purified on the large scale high pH MDAP (Method D)
  8. customthe solvent removed
  9. customThe resulting product was dried under high vacuum for 1 h

출처 및 근거

ORD 기록
ord-2889d8f517b3443fbbec5fa2fd6b9bc3
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633319B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트