Реакция #1509594
ord-8dbd5e9be6624a71b884402429269751
Уравнение реакции
[3-Amino-5-(1-methyl-1H-tetrazol-5-yl)-phenyl]-methanol
→
title compound
Выход 77.1%
3-Methyl-5-(1-methyl-1H-tetrazol-5-yl)-phenylamine
Выход 77.1%
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Другоеwas hydrogenated on a H-cube apparatus at 30° C.
- 2ДругоеAfter reaction completion
- 3Концентрированиеthe mixture was concentrated in vacuum
- 4ЭкстракцияThis was extracted with EtOAc
- 5Другоеthe organic layer was separated
- 6Другоеdried
- 7Концентрированиеconcentrated in vacuum
- 8ДругоеThe residue was purified by flash chromatography (98:2 DCM:MeOH)
Методика
A solution of [3-Amino-5-(1-methyl-1H-tetrazol-5-yl)-phenyl]-methanol (450 mg) in MeOH (20 ml) with a few drops of conc. HCl (aq) was hydrogenated on a H-cube apparatus at 30° C., and 10 bar with a flow rate of 1 mL/min using a Pd/C cartridge. After reaction completion, the mixture was concentrated in vacuum and the residue basified with a dilute K2CO3(aq). This was extracted with EtOAc and the organic layer was separated, dried and concentrated in vacuum. The residue was purified by flash chromatography (98:2 DCM:MeOH) to give the title compound (320 mg).