반응 #10192

ord-64bd259c84b24a4d881ac13f3981aa61

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과then filtered through a Celite pad
  2. 2
    농축concentrated to white solids (450 mg, 86%)

실험 절차

2,2,2-Trifluoro-1-(4-hydroxy-5-nitro-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-ethanone (575 mg, 1.82 mmol) was hydrogenated in methanol under a H2 atmosphere at (45 psi, or approximately 3 atmospheres) over 10% Pd/C (80 mg) for 1.5 hours then filtered through a Celite pad and concentrated to white solids (450 mg, 86%). (TLC 5% methanol/CH2Cl2 (NH3) Rf 0.6). 1H NMR (400 MHz, CD3OD) δ 6.67–6.59 (m, 2H), 4.12 (m, 1H), 3.73 (m, 1H), 3.73 (m, 1H), 3.51 (m, 1H), 3.07 (m, 2H), 2.24 (m, 1H), 1.94 (d, J=10.5 Hz, 1H). GCMS m/e 286 (M+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091372B2uspto-grants-2006_08