반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:14]2=[N:15][C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([N:24]4[CH2:27][CH:26]([OH:28])[CH2:25]4)=O)[C:17]=3[N:13]2[CH2:12][CH2:11][CH2:10]1.[B].O1CCCC1.[Cl-].[NH4+]>>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:14]2=[N:15][C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][N:24]4[CH2:27][CH:26]([OH:28])[CH2:25]4)[C:17]=3[N:13]2[CH2:12][CH2:11][CH2:10]1참가 물질
4
반응물 3
생성물 1
반응 조건
- 온도
- 70 °C
실험 절차
To a suspension of 1-{[1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]carbonyl}azetidin-3-ol (150 mg, 0.359 mmol) was added boron-tetrahydrofuran complex (1.0 M solution in tetrahydrofuran, 1.8 mL, 1.8 mmol), and the mixture was stirred at 70° C. for 13 hr. To the mixture was added aqueous saturated ammonium chloride, and the mixture was stirred at 70° C. for 20 min. The mixture was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give the solid, which was washed with ethanol to give the title compound as a colorless powder (91.5 mg, 0.227 mmol, 63%).
후처리
- stirringthe mixture was stirred at 70° C. for 20 min
- extractionThe mixture was extracted with ethyl acetate
- washThe combined organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give the solid, which
- washwas washed with ethanol
출처 및 근거
- ORD 기록
- ord-27e65e1702cb4679b55113cf36e13315
- 출처 데이터셋
- uspto-grants-2014_07
- 특허 번호
- US08785460B2
연결된 노트
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