反応式
[Cl:1][C:2]1[C:7]([CH:8]=C)=[CH:6][C:5]([C:10]#[N:11])=[CH:4][C:3]=1[NH:12][C:13]1[N:18]=[C:17]([NH:19][CH:20]2[CH2:22][CH2:21]2)[C:16]2=[N:23][CH:24]=[C:25]([C:26]#[N:27])[N:15]2[N:14]=1.O.I([O-])(=O)(=O)=[O:30].[Na+]>CC(C)=O.CC(O)(C)C.[Os]>[Cl:1][C:2]1[C:7]([CH:8]=[O:30])=[CH:6][C:5]([C:10]#[N:11])=[CH:4][C:3]=1[NH:12][C:13]1[N:18]=[C:17]([NH:19][CH:20]2[CH2:22][CH2:21]2)[C:16]2=[N:23][CH:24]=[C:25]([C:26]#[N:27])[N:15]2[N:14]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
A suspension of 2-((2-chloro-5-cyano-3-vinylphenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (Example 399) (210 mg, 0.557 mmol) in acetone (50 mL) was heated to give a cloudy solution. After cooling to room temperature; water (5 mL), osmium tertroxide (0.350 mL, 2.5 wt % in t-BuOH, 0.028 mmol) and sodium periodate (262 mg, 1.23 mmol) were added. After overnight stirring, additional water (20 mL) was added and the reaction was left stirring for 1 day. Most of the acetone was removed and the suspended solid was collected by filtration, washed with water, and air dried to leave 2-((2-chloro-5-cyano-3-formylphenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (188 mg) as a light yellow solid.
後処理
- temperaturewas heated
- customto give a cloudy solution
- waitthe reaction was left
- stirringstirring for 1 day
- customMost of the acetone was removed
- filtrationthe suspended solid was collected by filtration
- washwashed with water, and air
- customdried
出典と根拠
- ORDレコード
- ord-f57cb42b4e73433a8f17b3f3114bd499
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09273057B2
関連ノート
読み込み中…