反应详情

A solution with 2.91 g (12 mM) of crude 2-(4-methoxybenzyloxy)-2-methyl-propionyl chloride in 9 ml of THF was added within 90 min to a stirred suspension with 3.62 g (10 mM) of 5,6-diamino-1-(3-cyclopentyloxy-4-methoxy-benzyl)-2-thiouracil. After 20 hr another 485 mg of chloride in 5 ml of THF was added within 30 min. After a further 3 hr the solid was filtered off and the solution evaporated in vacuo to dryness. The residue was dissolved in ethyl acetate, extracted with sodium bicarbonate solution and the organic phase evaporated in vacuo to dryness. The residue was crystallized from methanol: 1.71 g (30.1%) of amide with mp 172-184° C.

1. filtrationAfter a further 3 hr the solid was filtered off
2. customthe solution evaporated in vacuo to dryness
3. dissolutionThe residue was dissolved in ethyl acetate
4. extractionextracted with sodium bicarbonate solution
5. customthe organic phase evaporated in vacuo to dryness
6. customThe residue was crystallized from methanol