반응 #2000563

ord-9d2acd63500c42fda6c8ec6c5f9299b7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed until a solution
  2. 2
    기타was obtained
  3. 3
    기타a white precipitate was formed
  4. 4
    여과The solution was filtered
  5. 5
    세척the precipitate washed with THF
  6. 6
    기타dried

실험 절차

5′-(5-Cyano-1-methyl-1H-pyrrol-2-yl)spiro[cyclohexane-1,3′-[3H]indol]-2′-ylidenecyanamide (16 g) in THF (100 mL) was treated with diethylamine (37 g) and refluxed until a solution was obtained. Upon cooling to ambient temperature, a white precipitate was formed. The solution was filtered, the precipitate washed with THF and dried to give 18.0 g (90% yield) of the diethylamine salt/complex. 1H NMR (DMSO-d6, ppm): 7.58, 7.21, 7.05, 7.00, 6.5-6 (br), 6.27, 3.71, 2.80 (q), 1.9-1.7, 1.5-1.4, and 1.10 (t).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08609712B2uspto-grants-2013_12