반응 #2264759

ord-d2d5b100715341eaa0d7dc69abb5de35

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at 100° C
  2. 2
    기타The crude reaction mixture
  3. 3
    농축was concentrated
  4. 4
    기타purified on 12 g SiO2 column with 0-10% NH3/MeOH CH2Cl2

실험 절차

A solution of Intermediate 2 (111 mg, 0.569 mmol) in AcOH (15 ml) was passed through a Rh/C catalyst cartridge on an H-Cube hydrogenation apparatus at a pressure of 80 bar and a flow rate of 1 ml/min at 100° C. The reaction was looped through the apparatus for 2 h. The crude reaction mixture was concentrated and purified on 12 g SiO2 column with 0-10% NH3/MeOH CH2Cl2 to give the desired compound (90 mg, 80%). MS (ESI): mass calcd. for C12H13N3, 199.3. m/z found, 200.2 [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09066946B2uspto-grants-2015_06