تفاعل #487513

ord-d2cbbf756b034feab2b4ccf2e794ccb4

معادلة التفاعل

[H-].[Na+]
Sodiumhydride
OCc1ccccc1
benzyl alcohol
OCc1ccccc1
benzyl alcohol
Clc1ncnc2nc[nH]c12
6-chloropurine
c1ccc(COc2ncnc3nc[nH]c23)cc1
6-Benzyloxypurine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىhas reached room temperature
  2. 2
    أخرى6-Benzyloxypurine was precipitated by the addition of acetic acid (4.6 ml) and diethylether (550 ml)
  3. 3
    أخرىThe precipitate was separated by filtration (11.72 g)
  4. 4
    أخرىRe-crystallization from ether gave (4.78 g; 65.4%)
  5. 5
    أخرىMelting point was 175-177° C. (lift. 170-172° C.)[Ramazaeva N., 1989 #473] 1H-NMR (DMSO-d6): 8.53 (1H, s); 8.39 (1H, s); 7.54-7.35 (5H, m); 5.62 (2H, s)

الإجراء التجريبي

Sodiumhydride (60% Dispersion in mineral oil; 3.23 g; 80 mmol) was slowly added to benzyl alcohol (30 ml; 34.7 mmol). After the addition of more benzyl alcohol (10 ml) and 6-chloropurine (5.36 g). The reaction mixture was heated to 100° C. for 4 hours. When the reaction mixture has reached room temperature, water (1 ml) was slowly added. 6-Benzyloxypurine was precipitated by the addition of acetic acid (4.6 ml) and diethylether (550 ml). The precipitate was separated by filtration (11.72 g). Re-crystallization from ether gave (4.78 g; 65.4%). Melting point was 175-177° C. (lift. 170-172° C.)[Ramazaeva N., 1989 #473] 1H-NMR (DMSO-d6): 8.53 (1H, s); 8.39 (1H, s); 7.54-7.35 (5H, m); 5.62 (2H, s).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08741566B2uspto-grants-2014_06