반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH:12]=[CH:13][N:14]=[C:7]1[C:6]([NH:15][CH2:16][CH2:17][CH2:18][OH:19])=[N:5]2.N12CCCN=C1CCCCC2.O=C1CCC(=O)N1[O:38][C:39](=O)[C@H:40]([NH:42][C:43](=[O:49])[O:44][C:45]([CH3:48])([CH3:47])[CH3:46])[CH3:41]>CN(C)C=O.O>[C:45]([O:44][C:43]([NH:42][C@H:40]([CH3:41])[C:39]([O:19][CH2:18][CH2:17][CH2:16][NH:15][C:6]1[C:7]2[N:8]([CH:12]=[CH:13][N:14]=2)[C:9]2[C:4]([N:5]=1)=[CH:3][C:2]([F:1])=[CH:11][CH:10]=2)=[O:38])=[O:49])([CH3:48])([CH3:47])[CH3:46]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 60 °C
실험 절차
To a solution of commercially available (Peakdale) 3-[(7-fluoroimidazo[1,2-a]quinoxalin-4-yl)amino]propan-1-ol (20 mg, 0.08 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (12 μL, 0.08 mmol) in anhydrous dimethylformamide (600 μL) under argon was added dropwise a solution of tert-butyl {(1R)-2-[(2,5-dioxopyrrolidin-1-yl)oxy]-1-methyl-2-oxoethyl}carbamate (22 mg, 0.08 mmol) in anhydrous dimethylformamide (200 μL). The mixture was stirred at 60° C. for 65 h, then diluted with cold water and extracted four times with chloroform and once with chloroform/isopropanol (5:1). The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated. The crude product was purified by preparative TLC (silica, dichloromethane/methanol 20/1) to afford the title compound as a colorless oil (4 mg, 12%).
후처리
- extractionextracted four times with chloroform
- washThe combined organic layers were washed with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- customThe crude product was purified by preparative TLC (silica, dichloromethane/methanol 20/1)
출처 및 근거
- ORD 기록
- ord-84aa437415f64c03aef66361a8453af1
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08513250B2
연결된 노트
불러오는 중…