反应详情

To a solution of the title product of Example 26 (0.493 g), 4-(dimethylamino)pyridine (0.226 g) and N,N-dimethylglycine hydrochloride (0.193 g) in 30 ml of CH2Cl2 was added a solution of dicyclohexylcarbodiimide in 5 ml of CH2Cl2. After stirring 18 hours, by-product dicyclohexyl urea was recovered by filtration and the filtrate stripped to an oily solid which was chromatographed on a silica gel column with ether as eluant to yield purified title product, 0.44 g. 1H-NMR(CDCl3)delta(ppm): 2.15 (s, 6H), 3.15 (s, 2H), 3.80 (s, 3H), 4.30 (d, J=5Hz, 2H), 4.90 (m, 1H), 6.30 (d, J=3, 1H), 6.30-8.30 (m, 13H).

1. filtrationby-product dicyclohexyl urea was recovered by filtration
2. customwas chromatographed on a silica gel column with ether as eluant
3. customto yield
4. custompurified title product, 0.44 g