反应详情

4N HCl/dioxane (1 ml) was added under ice cooling to (2R)-2-({cyclopropyl[4-methoxy-3-(3-methoxypropoxy)benzyl]amino}carbonyl)morpholin-4-carboxylic acid tert-butyl ester (a compound of Reference Example 8, 368 mg) dissolved in chloroform (4 ml), and the mixture was stirred at room temperature for 2 hours. Water was added to the mixture under ice cooling and the organic layer was separated. The aqueous layer was extracted with chloroform after being adjusted to pH 9 by addition of a saturated aqueous solution of sodium bicarbonate. The organic layer was washed with a saturated brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by NH-silica gel column chromatography (eluting solvent; n-hexane:ethyl acetate=1:1 to ethyl acetate only) to give (2R)—N-cyclopropyl-N-[4-methoxy-3-(3-methoxypropoxy)benzyl]morpholine-2-carboxamide (230 mg) as a colorless oil.

1. customthe organic layer was separated
2. extractionThe aqueous layer was extracted with chloroform
3. additionafter being adjusted to pH 9 by addition of a saturated aqueous solution of sodium bicarbonate
4. washThe organic layer was washed with a saturated brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by NH-silica gel column chromatography (
8. washeluting solvent