تفاعل #10538

ord-69e9be3268244ec6a9f9871f2e034f0a

المذيبات

ظروف التفاعل

درجة الحرارة
105°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىpurified by column chromatography on silica gel eluting with dichloromethane
  2. 2
    أخرىAfter evaporation of appropriate fractions the residue
  3. 3
    أخرىwas triturated with diethyl ether
  4. 4
    ترشيحfiltered
  5. 5
    أخرىdried

الإجراء التجريبي

A mixture of methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate (Preparation 9) (1.1 g, 2 mmol) and 1,2-ethylenediamine (1.1 g, 18.3 mmol) was heated at 105° C. for 2.5 hours. The mixture was dissolved in a little dichloromethane and purified by column chromatography on silica gel eluting with dichloromethane:methanol:concentrated aqueous ammonia (85:15:1.5, by volume). After evaporation of appropriate fractions the residue was triturated with diethyl ether, filtered and dried to yield the target compound as a white solid, (0.99 g, 86%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07094769B2uspto-grants-2006_08