تفاعل #68485

ord-d31892ae24954923a7f9c3f3201655b5

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was concentrated
  2. 2
    أخرىthen purified by MPLC chromatography (eluted with 0-10% methanol in dichloromethane)

الإجراء التجريبي

To a microwave vial (10-20 mL) was added (6-(3-methylisoxazol-5-yl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanamine (1.00 g, 4.34 mmol) and 8-chloro-3-methoxy-1,5-naphthyridine (1.10 g, 5.65 mmol) in 2-butanol (12 mL). The suspension was stirred at 120° C. under microwave irradiation for four hours. The mixture was concentrated and taken up in ammonia in methanol (2.0 M) then purified by MPLC chromatography (eluted with 0-10% methanol in dichloromethane) to yield the product as a tan solid. MS m/z=389.0 [M+1]+. Calc'd for C19H16N8O2: 388.1

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524900B2uspto-grants-2013_09