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

HRID 1036726ノート

反応式

HRID 1036726 の反応式
[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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8ccde26696944a359733b9d4fc5b15e0
出典データセット
uspto-grants-2013_10
特許番号
US08546416B2

反応ノート

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