三甲基硅烷化重氮甲烷 → 6-氨基-3-溴吡啶甲酸甲酯
反应方程式
[NH2:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([Br:11])=[CH:4][CH:3]=1.[Si](C=[N+]=[N-])(C)(C)[CH3:13]>C(OCC)(=O)C.CO>[NH2:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:13])=[O:9])[C:5]([Br:11])=[CH:4][CH:3]=1参与物
5
实验过程
To a solution of 6-amino-3-bromopicolinic acid (30 g) in ethyl acetate (300 mL) and methanol (300 mL) was added TMS-diazomethane (70 mL, 2M in hexanes) and the reaction mixture was stirred for 3 days. The mixture was concentrated, taken up in ether (500 mL) and washed with aqueous Na2CO3 solution (twice), then washed with brine, dried over sodium sulfate, filtered and concentrated to provide the title compound.
后处理
- concentrationThe mixture was concentrated
- washwashed with aqueous Na2CO3 solution (twice),
- washthen washed with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
来源与证据
- ORD记录
- ord-979721791f91448a8e687c1e4419bd9d
- 来源数据集
- uspto-grants-2016_01
- 专利号
- US09227963B2
反应笔记
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