反应详情

温度

75 °C

A flask was charged with sodium hydride (60% oil dispersion, 240 mg, ~6 mmol) which was washed with hexanes before the addition of isopropanol (20 mL) and (±)-cis-4-(2-amino-6-chloro-9H-purin-9-yl)-2-cyclopentene-1-methanol (0.318 g, 1.19 mmol) from Example 4. This solution was heated at 75° C. for 2 hours before being allowed to cool to room temperature and neutralized by addition of 1.0 N HC1. The solution was concentrated and the residue was placed on a silica gel column which was eluted with 10% methanol-chloroform. Crystallization from ethanol:water 1:1 yielded off-white crystals (265 mg, 77%), m.p. 188-191° C.

1. temperatureto cool to room temperature
2. additionneutralized by addition of 1.0 N HC1
3. concentrationThe solution was concentrated
4. washwas eluted with 10% methanol-chloroform
5. customCrystallization from ethanol:water 1:1 yielded off-white crystals (265 mg, 77%), m.p. 188-191° C.