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With m-chloroperoxybenzoic acid; 3-chloro-benzenecarboperoxoic acid In hydrogenchloride; water; 2,4-dichlorophenoxyacetic acid dimethylamine; toluene
EXAMPLE 1 8-Chloroadenine (1) To a solution of adenosine (2.67 g, 10 mmol) in DMA/HCl (0.5M, 45 mL) was added m-chloroperoxybenzoic acid (MCPBA, 3.22 g, 16 mmol 87percent) and stirred at room temperature for 2.5 h. An additional portion of MCPBA (0.9 g, 5 mmol) was added and stirring continued for another 1 h. Toluene (50 mL) was added to the reaction mixture and the solvents evaporated at 60° C. under vacuo to dryness. The residue was dissolved in water (50 mL) and extracted with ether (3*50 mL). The pH of the aqueous phase was adjusted to 5 with 2N NaOH and then diluted with EtOH (100 mL). The solution was stored in the refrigerator overnight. The light yellow solid that separated was collected, washed with cold EtOH (2*25 mL) and dried to give 1.44 g (85.2percent) of 1: mp 305°-310° C. (dec.) [Lit. mp>300° C. (dec.)]: IR (KBr): 630 (C-C1), 3100-3300 (NH2) cm-1: UV: λmax (pH 1) 262 nm (ε 8,700): λmax (pH 7) 268 nm (ε 7,900): λmax (pH 11) 269 nm (ε 8,300): 1 H NMR (Me2 SO-d6): δ 7.48 (br s, 2, NH2), 8.10 (s, 1, C2 H) and 13.60 (br s, 1, N9 H).
Reference：
[1] Patent: US4861873, 1989, A,
2
[ 17587-87-0 ]
[ 66224-66-6 ]
[ 28128-28-1 ]
Reference：
[1] Recueil: Journal of the Royal Netherlands Chemical Society, 1980, vol. 99, # 9, p. 267 - 270
With m-chloroperoxybenzoic acid; 3-chloro-benzenecarboperoxoic acid; In hydrogenchloride; water; 2,4-dichlorophenoxyacetic acid dimethylamine; toluene;
EXAMPLE 1 8-Chloroadenine (1) To a solution of adenosine (2.67 g, 10 mmol) in DMA/HCl (0.5M, 45 mL) was added m-chloroperoxybenzoic acid (MCPBA, 3.22 g, 16 mmol 87%) and stirred at room temperature for 2.5 h. An additional portion of MCPBA (0.9 g, 5 mmol) was added and stirring continued for another 1 h. Toluene (50 mL) was added to the reaction mixture and the solvents evaporated at 60 C. under vacuo to dryness. The residue was dissolved in water (50 mL) and extracted with ether (3*50 mL). The pH of the aqueous phase was adjusted to 5 with 2N NaOH and then diluted with EtOH (100 mL). The solution was stored in the refrigerator overnight. The light yellow solid that separated was collected, washed with cold EtOH (2*25 mL) and dried to give 1.44 g (85.2%) of 1: mp 305-310 C. (dec.) [Lit. mp>300 C. (dec.)]: IR (KBr): 630 (C-C1), 3100-3300 (NH2) cm-1: UV: lambdamax (pH 1) 262 nm (epsilon 8,700): lambdamax (pH 7) 268 nm (epsilon 7,900): lambdamax (pH 11) 269 nm (epsilon 8,300): 1 H NMR (Me2 SO-d6): delta 7.48 (br s, 2, NH2), 8.10 (s, 1, C2 H) and 13.60 (br s, 1, N9 H).
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