Trifluoroacetic acid → 4-(4-Fluorophenyl)-2-((5-methylisoxazol-3-yl)methyl)-2,7-diazaspiro[4.5]decan-1-one

HRID 1036726노트

반응식

HRID 1036726 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:12]3([CH2:17][CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13]3)[C:11](=[O:25])[N:10]([CH2:26][C:27]3[CH:31]=[C:30]([CH3:32])[O:29][N:28]=3)[CH2:9]2)=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:12]3([CH2:17][CH2:16][CH2:15][NH:14][CH2:13]3)[C:11](=[O:25])[N:10]([CH2:26][C:27]3[CH:31]=[C:30]([CH3:32])[O:29][N:28]=3)[CH2:9]2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 71060659Tert-butyl 4-(4-fluorophenyl)-2-((5-methylisoxazol-3-yl)methyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate

생성물 1

HCID 710604374-(4-Fluorophenyl)-2-((5-methylisoxazol-3-yl)methyl)-2,7-diazaspiro[4.5]decan-1-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Tert-butyl 4-(4-fluorophenyl)-2-((5-methylisoxazol-3-yl)methyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate (243.6 mg; 0.549 mmol) was solubilised in DCM (1 ml). Trifluoroacetic acid (0.86 ml; 11.14 mmol) was added and the mixture stirred at RT for 20 minutes before being concentrated in vacuo. The oil was dissolved with methanol (5 ml) and passed through a 10 g SCX-2 cartridge eluting with 2M NH3 in methanol (50 ml) and concentrated in vacuo to yield the title compound.

후처리

  1. concentrationbefore being concentrated in vacuo
  2. dissolutionThe oil was dissolved with methanol (5 ml)
  3. washeluting with 2M NH3 in methanol (50 ml)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8ccde26696944a359733b9d4fc5b15e0
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546416B2

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