反応 #1509594

反応方程式

[3-Amino-5-(1-methyl-1H-tetrazol-5-yl)-phenyl]-methanol

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title compound

収率 77.1%

3-Methyl-5-(1-methyl-1H-tetrazol-5-yl)-phenylamine

収率 77.1%

溶媒

MeOH

反応条件

後処理

1. 1
   その他was hydrogenated on a H-cube apparatus at 30° C.
2. 2
   その他After reaction completion
3. 3
   濃縮the mixture was concentrated in vacuum
4. 4
   抽出This was extracted with EtOAc
5. 5
   その他the organic layer was separated
6. 6
   その他dried
7. 7
   濃縮concentrated in vacuum
8. 8
   その他The residue was purified by flash chromatography (98:2 DCM:MeOH)

実験手順

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).

出典