반응식
[I:1][C:2]1[N:11]=[CH:10][C:9]2[CH2:8][CH2:7][C:6]3[C:12]([C:16]([O:18]CC)=O)=[N:13][N:14]([CH3:15])[C:5]=3[C:4]=2[N:3]=1.[OH-].[K+].C(N(C(C)C)C(C)C)C.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[CH2:54]([C:56]1[CH:62]=[CH:61][CH:60]=[C:59]([CH2:63][CH3:64])[C:57]=1[NH2:58])[CH3:55]>C(O)C>[CH2:54]([C:56]1[CH:62]=[CH:61][CH:60]=[C:59]([CH2:63][CH3:64])[C:57]=1[NH:58][C:16]([C:12]1[C:6]2[CH2:7][CH2:8][C:9]3[CH:10]=[N:11][C:2]([I:1])=[N:3][C:4]=3[C:5]=2[N:14]([CH3:15])[N:13]=1)=[O:18])[CH3:55]참가 물질
반응물 5
생성물 1
시약·촉매·용매 1
실험 절차
Ethyl 8-iodo-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate (4.0 g, 10.4 mmol) prepared as described in WO2004/104007 was dissolved in anhydrous ethanol (150 mL) and treated with potassium hydroxide (5.83 g, 104 mmol.) at RT for 24 hour. The white precipitate formed during the reaction was collected by filtration. The solid was then suspended in anhydrous dimethylformamide (5.0 mL) and treated with N-ethyl-N,N-diisopropylamine (10 ml) and O-(Benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TBTU) (4.5 g, 14.1 mmol). The mixture was then treated with 2,6-diethylaniline (2.3 ml, 14.1 mmol) and stirred at room temperature overnight. The solvent was removed under reduced pressure and the crude was purified by column chromatography to afford the title compound.
후처리
- customThe white precipitate formed during the reaction
- filtrationwas collected by filtration
- customThe solvent was removed under reduced pressure
- customthe crude was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-059465ba97fd4bd59d5555eae22fd6f4
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846701B2
연결된 노트
불러오는 중…