反应详情

200 μl of a 4N dioxane solution of hydrogen chloride were added to a solution of 339 mg (0.54 mmol) of N-(2-t-butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide [prepared as described in step (i) above] in 3 ml of diethyl ether, and the crystals which precipitated were collected by filtration and washed with diethyl ether. The crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm) using a 3:1 by volume mixture of acetonitrile and water as the eluent, to give a gel. This gel was crystallized by trituration with diethyl ether, to give 170 mg (yield 85%) of the title compound as colorless crystals, melting at 125°-133° C.

1. customthe crystals which precipitated
2. filtrationwere collected by filtration
3. washwashed with diethyl ether
4. customThe crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm)
5. additionby volume mixture of acetonitrile and water as the eluent
6. customto give a gel
7. customThis gel was crystallized by trituration with diethyl ether