반응 #837165

ord-976efe83d7944f0ab6866d25146c10a0

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed in vacuo

실험 절차

To the product from step 1 (70 mg, 0.183 mmol) was added 4M HCl in dioxane (6 mL) and the resulting mixture was stirred at rt for 3 h. The solvent was removed in vacuo to obtain the product as a brown solid, (51 mg, 99%): MS, m/z 282 (M+H): LCMS (UV) 99%: HPLC 98.3%; 1H NMR (400 MHz, DMSO-d6) δ 1.72-1.81 (m, 1H), 1.89-2.00 (m, 2H), 2.02-2.19 (m, 1H), 3.19-3.26 (m, 2H), 3.91-3.98 (m, 1H), 4.25-4.30 (dd, 1H J1=8.4 Hz, J2=10.8 Hz), 4.36-4.40 (dd, 1H J1=3.6 Hz, J2=10.8 Hz), 7.15 (d, 2H, J=9.2 Hz), 7.54-7.59 (m, 2H), 7.65-7.71 (m, 3H); 7.785 (d, 2H, J=8.8 Hz), 9.4 (s, 2H)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07402684B2uspto-grants-2008_07