반응 #1095869

ord-04f37ee08a704638b9cb3bf1fe497305

반응 방정식

CC1CCCCN1
2-methylpiperidine
CN(C)C=O
N,N-dimethylformamide
CC#CCOc1cc(Cl)ncn1
4-chloro-6-(2-butynyloxy)pyrimidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC#CCOc1cc(N2CCCCC2C)ncn1
4-(2-butynyloxy)-6-(2-methylpiperidino)pyrimidine
수율 27.0%

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    온도The reaction mixture was cooled to near room temperature
  3. 3
    세척the mixture was washed with a saturated sodium chloride aqueous solution three times
  4. 4
    건조The organic layers were dried over anhydrous magnesium sulfate
  5. 5
    농축concentrated

실험 절차

Into 2 ml of N,N-dimethylformamide was resolved 183 mg of 4-chloro-6-(2-butynyloxy)pyrimidine, 166 mg of potassium carbonate and 99 mg of 2-methylpiperidine was added therein, and the mixture was stirred for 4 hours at 80° C. and 3 hours at 120° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 66 mg of 4-(2-butynyloxy)-6-(2-methylpiperidino)pyrimidine (hereinafter, referred to as Compound (20)).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07973028B2uspto-grants-2011_07