تفاعل #6346

ord-b7ee7fbacb394ae7a8be509b810a5cae

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling the suspension
  2. 2
    أخرىwas evaporated to dryness
  3. 3
    أخرىthe residue partitioned between chloroform (750 ml) and water (500 ml)
  4. 4
    غسيلThe separated aqueous phase was washed with chloroform (200 ml)
  5. 5
    غسيلThe combined organic phases were washed with water
  6. 6
    تجفيفdried (MgSO4)
  7. 7
    أخرىevaporated
  8. 8
    أخرىaffording an orange solid homogeneous on t.l.c

الإجراء التجريبي

A solution of 9-benzyloxy-6-chloropurine (38.4 g; 0.147 mmol) in ethanol (300 ml) saturated with ammonia was heated at 100° C. in an autoclave for 16 hours. After cooling the suspension was evaporated to dryness and the residue partitioned between chloroform (750 ml) and water (500 ml). The separated aqueous phase was washed with chloroform (200 ml). The combined organic phases were washed with water, dried (MgSO4) and evaporated, affording an orange solid homogeneous on t.l.c. (31.1 g, 87%). IR: νmax (KBr) 3372, 3300, 3187, 3038, 1660, 1637, 1600, 1581 cm-1 ; 1H NMR: δH [(CD3)2SO] 5.3(2H, s, CH2Ar), 6.8(2H, br.s, D2O exchangeable, NH2), 7.3(6H, s, H-8, Ar), 7.7(1H, s, H-2). Found: C, 59.39; H, 4.60; N, 29.07%; m/e 241 0949. C12H11N5O requires: C, 59.73; H, 4.60; N, 29.03%; m/z 241.0964.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05247085uspto-grants-1993_09