10-Azetidin-1-yl-3-pyridin-2-ylethynyl-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester → 10-Azetidin-1-yl-3-(2-pyridin-2-yl-ethyl)-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:33][CH2:32][C:12]2=[C:13]([N:28]3[CH2:31][CH2:30][CH2:29]3)[N:14]3[C:18]([N:19]=[C:11]2[CH2:10][CH2:9]1)=[C:17]([C:20]#[C:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[CH:16]=[N:15]3)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[OH-].[Pd+2].[OH-]>[C:1]([O:5][C:6]([N:8]1[CH2:33][CH2:32][C:12]2=[C:13]([N:28]3[CH2:31][CH2:30][CH2:29]3)[N:14]3[C:18]([N:19]=[C:11]2[CH2:10][CH2:9]1)=[C:17]([CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[CH:16]=[N:15]3)=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
4
反応物 1
生成物 1
試薬・触媒・溶媒 2
実験手順
To 87 mg (0.2 mmol) 10-azetidin-1-yl-3-pyridin-2-ylethynyl-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester in 3 mL ethanol was added 11 mg (20% weight) palladium hydroxide, the reaction was purged 3 times with nitrogen then 3 times with hydrogen and was stirred at room temperature under a balloon of hydrogen for 16 hours. The mixture was purged twice with nitrogen, then the solution was filtered through a pad of celite. After evaporation of the solvent the product was purified by column chromatography (silica, heptane/EtOAc 9:1 to 3:7).
後処理
- customthe reaction was purged 3 times with nitrogen
- customThe mixture was purged twice with nitrogen
- filtrationthe solution was filtered through a pad of celite
- customAfter evaporation of the solvent the product
- customwas purified by column chromatography (silica, heptane/EtOAc 9:1 to 3:7)
出典と根拠
- ORDレコード
- ord-63f65218df754bbeb63f46cdff7da24e
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09346816B2
反応ノート
読み込み中…