반응 #6346

반응 방정식

KBr

9-benzyloxy-6-chloropurine

ammonia

→

9-Benzyloxyadenine

용매

ethanol

반응 조건

후처리

1. 1
   온도After cooling the suspension
2. 2
   기타was evaporated to dryness
3. 3
   기타the residue partitioned between chloroform (750 ml) and water (500 ml)
4. 4
   세척The separated aqueous phase was washed with chloroform (200 ml)
5. 5
   세척The combined organic phases were washed with water
6. 6
   건조dried (MgSO4)
7. 7
   기타evaporated
8. 8
   기타affording an orange solid homogeneous on t.l.c

실험 절차

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.

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