反应方程式
[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]1参与物
4
反应条件
- 温度
- 70 °C
实验过程
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%).
后处理
- 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
来源与证据
- ORD记录
- ord-d0a01f1bfd2248ec8502512630dbb024
- 来源数据集
- uspto-grants-2014_12
- 专利号
- US08901141B2
关联笔记
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