반응 #51616

ord-60dc820a1ebd4013beebac37a1fde919

반응 방정식

COc1cc2ncc(Cl)nc2cc1OC
2-chloro-6,7-dimethoxyquinoxaline
NC1CCCCC1
cyclohexylamine
COc1cc2ncc(NC3CCCCC3)nc2cc1OC
product
수율 69.0%
COc1cc2ncc(NC3CCCCC3)nc2cc1OC
2-cyclohexylamino-6,7-dimethoxyquinoxaline
수율 69.0%

반응 조건

온도
135°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mix is partitioned between CH2Cl2 and saturated NaHCO3
  2. 2
    건조The organic layer is dried (MgSO4)
  3. 3
    농축concentrated
  4. 4
    기타The resulting syrup is chromatographed (1:1 EtOAc:CH2Cl2)

실험 절차

To 0.3 g (1.34 mmol) of 2-chloro-6,7-dimethoxyquinoxaline is added approx. 1 mL of cyclohexylamine. The mixture is heated overnight at 105° C. and a further 10 hours at 135° C. The mix is partitioned between CH2Cl2 and saturated NaHCO3. The organic layer is dried (MgSO4) and concentrated. The resulting syrup is chromatographed (1:1 EtOAc:CH2Cl2) to provide 0.265 g of the product as a lt. brown solid in 69% yield (m.p. 188-189.5). Anal. calcd for C16H21N3O2: C, 66.88; H, 7.37; N, 14.62. Found: C, 66.82; H, 7.28; N, 14.45.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06852712B2uspto-grants-2005_02