反応式
[N:1]([CH2:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[N:10]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[N:9]=[C:8]2[C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=1)=[N+]=[N-]>C(O)C.O1CCCC1.C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-]>[NH2:1][CH2:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[N:10]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[N:9]=[C:8]2[C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=1参加物
5
反応物 1
生成物 1
試薬・触媒・溶媒 3
実験手順
To a solution of 550 mg of tert-butyl 5-(azidomethyl)-3-(3-fluorophenyl)-1H-1-indazolecarboxylate in a mixture of 10 ml ethanol and 5 ml tetrahydrofuran was added 110 mg of 5% palladium-calcium carbonate, and the mixture was hydrogenated at room temperature at normal pressure for 1.5 hours. After filtering off the catalyst through Celite, the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:methanol=1:0 to 9:1), to give 427 mg of the title compound as light green crystals.
後処理
- filtrationAfter filtering off the catalyst through Celite
- customthe solvent was evaporated
- customThe crude product was purified
- customseparated by silica gel column chromatography (ethyl acetate:methanol=1:0 to 9:1)
出典と根拠
- ORDレコード
- ord-08ccff159818498d9a4ea4f0971a21ed
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07776890B2
関連ノート
読み込み中…