반응식
[N:1]1[C:10]2[C:5](=[CH:6][C:7]([CH2:11][N:12]3[C:16]4=[N:17][C:18]([N:21]5[CH2:25][CH2:24][C:23](=O)[CH2:22]5)=[CH:19][N:20]=[C:15]4[N:14]=[N:13]3)=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.FC1(F)CC[NH:30][CH2:29]1>O1CCCC1.CO.CC(N(C)C)=O>[CH3:29][NH:30][C@@H:23]1[CH2:24][CH2:25][N:21]([C:18]2[N:17]=[C:16]3[N:12]([CH2:11][C:7]4[CH:6]=[C:5]5[C:10](=[CH:9][CH:8]=4)[N:1]=[CH:2][CH:3]=[CH:4]5)[N:13]=[N:14][C:15]3=[N:20][CH:19]=2)[CH2:22]1참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 80 °C
실험 절차
A suspension of 1-[1-(quinolin-6-ylmethyl)-1H-[1,2,3]triazolo[4,5-b]pyrazin-6-yl]pyrrolidin-3-one (50 mg, 0.15 mmol) and 3,3-difluoropyrrolidine (42 mg, 0.29 mmol) in tetrahydrofuran/methanol/dimethylacetamide (1.0 mL each) was heated to 80° C. for 2 hours then NaBCNH3 (18 mg, 0.29 mmol) was added. After 2 hours the solution was cooled to room temperature and concentrated. The crude product was purified by flash chromatography using a Horizon purification system on a 25S column eluting with chloroform/acetone (5-50%) followed by a second column on a 12M cartridge eluting with chloroform/ethyl acetate (25-100%) to afford the title compound (25 mg, 40%).
후처리
- additionNaBCNH3 (18 mg, 0.29 mmol) was added
- temperatureAfter 2 hours the solution was cooled to room temperature
- concentrationconcentrated
- customThe crude product was purified by flash chromatography
- customa Horizon purification system on a 25S column
- washeluting with chloroform/acetone (5-50%)
- washeluting with chloroform/ethyl acetate (25-100%)
출처 및 근거
- ORD 기록
- ord-5c3e3bb1ce0c4d1096cbf35ede4881e8
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07732604B2
연결된 노트
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