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, φ 30 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, φ 30 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