反应详情

To a stirred solution of 2,6-dichloropurine (500 mg, 2.64 minol) in acetonitrile (40 mL)at -10° C. was added 18-crown-6 (48 mg, 0.18 mmol) and potassium hydride (106 mg after ether wash of 35% dispersion in mineral oil, 2.64 mmol). The reaction was allowed to warm to room temperature and stirred for an additional 30 min. 4-Bromomethyl-N-methyl-N-cyclohexyl benzamide (900 mg, 2.90 mmol) was added in small amounts over 10 min and the mixture stirred under argon at 25° C. After 18 hr, the reaction was quenched by adding drops of acetic acid and the solvent removed under reduced pressure at <45° C. The residue was dissolved in ethyl acetate and washed with aqueous potassium carbonate, water and brine. The solvent was removed and the crude mixture (1.28 g) chromatographed (silica gel, CH2Cl2 /MeOH 100/7) to give pure 6A (278 mg, 25%). m.p. 134°-136° C. Anal calcd. for C20H21N5OCl2.0.25 H2O:C, 56.80; H, 5.08; N, 16.56; Cl, 16.80. Found: C, 57.00; H, 5.09; N, 16.20; Cl, 16.59.

1. stirringthe mixture stirred under argon at 25° C
2. waitAfter 18 hr
3. customthe reaction was quenched
4. additionby adding drops of acetic acid
5. customthe solvent removed under reduced pressure at <45° C
6. dissolutionThe residue was dissolved in ethyl acetate
7. washwashed with aqueous potassium carbonate, water and brine
8. customThe solvent was removed
9. customthe crude mixture (1.28 g) chromatographed (silica gel, CH2Cl2 /MeOH 100/7)