تفاعل #46362

ord-e387087c8a394279bd035d0d571cc60a

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    أخرىthe reaction solution was partitioned between ethyl acetate and water
  3. 3
    غسيلThe organic layer was washed with water, saturated brine
  4. 4
    أخرىdried
  5. 5
    أخرىevaporated
  6. 6
    أخرىThe residue was chromatographed over silica gel
  7. 7
    غسيلeluting with a gradient of 10 to 50% ethyl acetate in hexane

الإجراء التجريبي

(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (1.14 g), and 2-chloro-6,7-difluoro-3-methylquinoxaline Teng et al PCT Int. Appl (2000), WO00/42026A1 20000720 (1.14 g) were dissolved in DMF (2 ml) and heated to 90° C. for 3 days under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with water, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 10 to 50% ethyl acetate in hexane. The title compound was obtained as a pink foam (0.524 g), MH+ 393.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741329B2uspto-grants-2010_06