반응 #42634

ord-2f59057de17345809ee82ef0e8995252

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the precipitate was filtered
  2. 2
    세척washed several times with water
  3. 3
    기타dried

실험 절차

2-Thiophenecarbonylchloride (2.04 g, 1.49 mL) was added to a solution of tert-butyl-1-piperazinecarboxylate (2.5 g, 13.4 mmol) and DMAP (20 mg) in pyridine (15 mL) at 0° C. under N2 atmosphere and stirred at room temperature for overnight. The mixture was poured into ice water, the precipitate was filtered, washed several times with water, and dried to yield white solids (3.5 g, 88%). Mp 76° C. 1H NMR (DMSO-d6): δ 1.42 (s, 12H), 3.40 (m, 4H), 3.61 (m, 4H), 7.12 (m, 1H), 7.43 (d, J=4.1 Hz, 1H), 7.77 (d, J=4.8 Hz, 1H). EIMS m/z 297 (M+1), 319 (M+23). Anal. (C14H20N2O3S) C, H, N.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732146B2uspto-grants-2010_06