반응 #58764

ord-19f1fe01c2814fc19ddfc1b7a34455c7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축was concentrated
  2. 2
    기타to yield the crude product (0.140 g)
  3. 3
    기타The crude product was purified (SiO2: 0-5% 2 M NH3 in MeOH/DCM)

실험 절차

1-[3-(5-Chloromethyl-isoxazol-3-yloxy)-propyl]-piperidine (0.15 g, 0.80 mmol) was dissolved in DCM (5 mL) and piperidine (0.24 mL, 2.4 mmol) was added slowly. The reaction mixture was stirred overnight at rt and then was concentrated to yield the crude product (0.140 g). The crude product was purified (SiO2: 0-5% 2 M NH3 in MeOH/DCM) to give the final product (0.118 g, 47.6%). MS (ESI): exact mass calcd. for C17H29N3O2, 307.23; m/z found 308.4 [M+H]+. 1H NMR (500 MHz, CDCl3): 5.75 (s, 1H), 4.25-4.20 (m, 2H), 3.53 (s, 2H), 2.47-2.31 (m, 10H), 1.98-1.90 (m, 2H), 1.61-1.52 (m, 8H), 1.45-1.35 (m, 4H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423147B2uspto-grants-2008_09