تفاعل #1095880

ord-f738ecfc958e42c4a75a6e21af3def39

معادلة التفاعل

[Cl-].[NH4+]
ammonium chloride
CC#CCOc1cc(Cl)ncn1
4-(2-butynyloxy)-6-chloropyrimidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC1(C)CCCNC1.Cl
3,3-dimethylpiperidine hydrochloride
CC#CCOc1cc(N2CCCC(C)(C)C2)ncn1
4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine
المردود 95.1%

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was cooled to near room temperature
  2. 2
    استخلاصthe mixture was extracted with tert-butyl methyl ether three times
  3. 3
    غسيلThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated

الإجراء التجريبي

Into 2 ml of acetonitrile were added 0.20 g of 4-(2-butynyloxy)-6-chloropyrimidine, 0.45 g of potassium carbonate and 0.20 g of 3,3-dimethylpiperidine hydrochloride, and the mixture was stirred for 2 hours at 80° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.27 g of 4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine (hereinafter, referred to as Compound (31)).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07973028B2uspto-grants-2011_07