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

tert-butyl 3-{[3'-fluoro-4'-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoate → 3-{[3'-fluoro-4'-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoic acid

HRID 1026561
노트
인쇄 미리보기

반응식

HRID 1026561 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[O:35][CH2:36][C:37]([CH3:46])([CH3:45])[C:38]([O:40]C(C)(C)C)=[O:39])[CH:5]=[CH:6][C:7]=1[C:8]([N:10]1[CH2:15][CH2:14][CH:13]([N:16]2[C:21](=[O:22])[C@H:20]([CH3:23])[O:19][C:18]3[N:24]=[CH:25][C:26]([F:28])=[CH:27][C:17]2=3)[CH2:12][CH2:11]1)=[O:9]>FC(F)(F)C(O)=O>[F:1][C:2]1[CH:3]=[C:4]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[O:35][CH2:36][C:37]([CH3:45])([CH3:46])[C:38]([OH:40])=[O:39])[CH:5]=[CH:6][C:7]=1[C:8]([N:10]1[CH2:15][CH2:14][CH:13]([N:16]2[C:21](=[O:22])[C@H:20]([CH3:23])[O:19][C:18]3[N:24]=[CH:25][C:26]([F:28])=[CH:27][C:17]2=3)[CH2:12][CH2:11]1)=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 68005985tert-butyl 3-{[3'-fluoro-4'-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoate

생성물 1

HCID 680063803-{[3'-fluoro-4'-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoic acid수율 77.9%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A trifluoroacetic acid solution (10 ml) of tert-butyl 3-{[3′-fluoro-4′-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoate (940 mg) was stirred at room temperature for 1 hour. After the reaction solution was concentrated under reduced pressure, the resulting residue was neutralized with a saturated aqueous sodium hydrogen carbonate solution, and then a 10% aqueous citric acid solution was added, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. Ethyl acetate-hexane was added to the residue to collect the precipitate by filtration. This was redissolved in ethanol, to which water was added, and the resulting precipitate was collected by filtration to afford 3-{[3′-fluoro-4′-({4-[(3S)-7-fluoro-3-methyl-2-oxo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-1-yl]piperidin-1-yl}carbonyl)biphenyl-2-yl]oxy}-2,2-dimethylpropanoic acid (668 mg).

후처리

  1. concentrationAfter the reaction solution was concentrated under reduced pressure
  2. additiona 10% aqueous citric acid solution was added
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionEthyl acetate-hexane was added to the residue
  7. customto collect the precipitate
  8. filtrationby filtration
  9. dissolutionThis was redissolved in ethanol, to which water
  10. additionwas added
  11. filtrationthe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-43101316889e47fea665c13e5fd9289b
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729095B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트