반응 #1509594

ord-8dbd5e9be6624a71b884402429269751

반응 방정식

Cn1nnnc1-c1cc(N)cc(CO)c1
[3-Amino-5-(1-methyl-1H-tetrazol-5-yl)-phenyl]-methanol
Cc1cc(N)cc(-c2nnnn2C)c1
title compound
수율 77.1%
Cc1cc(N)cc(-c2nnnn2C)c1
3-Methyl-5-(1-methyl-1H-tetrazol-5-yl)-phenylamine
수율 77.1%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was hydrogenated on a H-cube apparatus at 30° C.
  2. 2
    기타After reaction completion
  3. 3
    농축the mixture was concentrated in vacuum
  4. 4
    추출This was extracted with EtOAc
  5. 5
    기타the organic layer was separated
  6. 6
    기타dried
  7. 7
    농축concentrated in vacuum
  8. 8
    기타The residue was purified by flash chromatography (98:2 DCM:MeOH)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045323E1uspto-grants-2015_01