تفاعل #472801

ord-3d3f9e4a43f94f09abe95102df6e0cdd

المذيبات

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    درجة الحرارةthe mixture was heated
  3. 3
    درجة الحرارةunder reflux
  4. 4
    ترشيحthe solid was filtered off

الإجراء التجريبي

To a suspension of 0.30 g of tert-butyl (2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)(1-(2-(7-fluoro-2-oxo-1,5-naphthyridin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate in 1.8 mL of isopropyl alcohol, 0.23 mL of concentrated hydrochloride was added, and the mixture was heated under reflux while stirring for 1 hour 50 minutes. The reaction mixture was cooled to 5° C., and the solid was filtered off to obtain 0.28 g of 1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)piperidin-1-yl)ethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one trihydrochloride as a light yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08367831B2uspto-grants-2013_02