反应详情

Methyl 2-methoxy-5-nitrobenzoate (10 g, 47.39 mmol) and hydroxylamine hydrochloride (13.17 g, 189.56 mmol) were taken up in MeOH (100 ml) and a solution of KOH (13.27 g, 236.95 mmol) in MeOH (55 ml) was added carefully. Note—an exothermic reaction was observed; solids initially dissolved, then a solid precipitated out of solution. TLC (run in EtOAc) of an acid washed aliquot showed a trace of the starting benzoate and a new product. H2O (100 ml) was added and any undissolved solid collected by filtration off, washed with isopropyl alcohol (IPA) and dried in vacuo to give 10.23 g (>100%) of N-hydroxy-2-methoxy-5-nitrobenzamide as a white solid.

1. customreaction
2. dissolutionsolids initially dissolved
3. customa solid precipitated out of solution
4. washTLC (run in EtOAc) of an acid washed aliquot
5. additionH2O (100 ml) was added
6. filtrationany undissolved solid collected by filtration off,
7. washwashed with isopropyl alcohol (IPA)
8. customdried in vacuo