Piperidine → HCID 178456792、化合物
反応式
[NH:1]1[CH2:7][C:5](=[O:6])[NH:4][C:2]1=[O:3].[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([F:37])=[C:13]([NH:15][C:16]2[CH:21]=[C:20]([NH:22][CH2:23][CH:24]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)[CH3:25])[N:19]3[N:32]=[CH:33][C:34]([CH:35]=O)=[C:18]3[N:17]=2)[CH:14]=1.N1CCCCC1>C(O)C.O>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([F:37])=[C:13]([NH:15][C:16]2[CH:21]=[C:20]([NH:22][CH2:23][CH:24]([N:26]3[CH2:27][CH2:28][O:29][CH2:30][CH2:31]3)[CH3:25])[N:19]3[N:32]=[CH:33][C:34]([CH:35]=[C:7]4[NH:1][C:2](=[O:3])[NH:4][C:5]4=[O:6])=[C:18]3[N:17]=2)[CH:14]=1参加物
6
反応条件
- 温度
- 80 °C
実験手順
Hydantoin (7 mg, 0.07 mmol) and 5-(5-chloro-2-fluorophenylamino)-7-(2-morpholinopropylamino)pyrazolo[1,5-a]pyrimidine-3-carbaldehyde (15 mg, 0.035 mmol) were dissolved in ethanol (0.5 mL) along with piperidine (7 uL, 0.07 mmol). The reaction was heated at 80° C. for 1 hour in the microwave. The reaction was then cooled to r.t., diluted with water, and the precipitate was collected and washed with water, 1:1 ethanol:water, then ethanol. The yellow solid was dried in vacuo to give 5-((5-(5-chloro-2-fluorophenylamino)-7-(2-morpholinopropylamino)pyrazolo[1,5-a]pyrimidin-3-yl)methylene)imidazolidine-2,4-dione (5 mg, 28% yield). LCMS (M+1=515)
後処理
- temperatureThe reaction was then cooled to r.t.
- customthe precipitate was collected
- washwashed with water, 1:1 ethanol
- customThe yellow solid was dried in vacuo
出典と根拠
- ORDレコード
- ord-d0a88b14df7b496e866ac50e8dbe9390
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08575177B2
反応ノート
読み込み中…