تفاعل #309564

ord-0e554514373a4c33948e8fece97d9aa8

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe reaction batch is filtered
  2. 2
    أخرىevaporated
  3. 3
    أخرىPurification of the residue by column chromatography on silica gel (eluent: petroleum ether: ethyl acetate 7:3)

الإجراء التجريبي

4.2 2.50 g of tert-butyl 3-tert-butoxycarbonylamino-6-ethoxy-7-fluoro-5-nitroindazole-1-carboxylate are hydrogenated in 20 ml of methanol at RT (catalyst: Raney nickel 0.5 g, hydrogen uptake: 300 ml). The reaction batch is filtered and evaporated. Purification of the residue by column chromatography on silica gel (eluent: petroleum ether: ethyl acetate 7:3) gives 3.30 g (36%) of tert-butyl 5-amino-3-tert-butoxycarbonylamino-6-ethoxy-7-fluoroindazole-1-carboxylate, MS-FAB (M+H+)=441.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08207210B2uspto-grants-2012_06