Trifluoroacetic acid methylene chloride → N-(4-fluoro-2-methylphenyl)azetidin-3-amine
反应方程式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)=[C:4]([CH3:20])[CH:3]=1.FC(F)(F)C(O)=O.ClCCl>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:12][NH:11][CH2:10]2)=[C:4]([CH3:20])[CH:3]=1参与物
4
实验过程
To an ice cooled solution of tert-butyl 3-((4-fluoro-2-methylphenyl)amino)azetidine-1-carboxylate (D30) (300 mg, 1.07 mmol) in dichloromethane (2 ml), a mixture of trifluoroacetic acid/dichloromethane (4.5 ml/1.5 ml) was added and the mixture stirred at room temperature for 1 h. Solvents were evaporated in vacuo and the resulting residue was purified by SPE-SCX cartridge (10 g). Collected ammonia fractions, after solvent evaporation afforded the title compound (D55) (0022/107/1) (190 mg)
后处理
- additionwas added
- customSolvents were evaporated in vacuo
- customthe resulting residue was purified by SPE-SCX cartridge (10 g)
- customCollected ammonia fractions, after solvent evaporation
来源与证据
- ORD记录
- ord-5184a9bd74214ac4abe69de265c0ac4e
- 来源数据集
- uspto-grants-2014_09
- 专利号
- US08828987B2
反应笔记
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