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温度

0 °C

To a solution of 1,3-dibenzyl barbituric acid 192 mg (0.623 mmol) in dry dichloromethane 2.0 mL under nitrogen atmosphere, added was pyridine 1.0 mL (12 mmol) and stirred at 0° C. Added was phenylacetyl chloride 96 mg (0.623 mmol, 1.00 equivalent) in dichloromethane 1.0 mL to the solution slowly during a period of 20 minutes, then stirred at room temperature for 3 hours. Added was dichloromethane 40 mL and washed the organic layer with 2 M hydrochloric acid and saturated brine, and dried over sodium sulfate. Purified was the crude product 273 mg, after removal of the solvent under the reduced pressure, by column chromatography (silica gel, eluted with dichloromethane). It obtained 1,3-dibenzyl-5-(phenylacetyl)barbituric acid 236 mg as colorless viscous oil at first (88.7% yield) and it gradually turned white plates.

1. additionAdded
2. customof 20 minutes
3. stirringstirred at room temperature for 3 hours
4. additionAdded
5. washwashed the organic layer with 2 M hydrochloric acid and saturated brine
6. dry with materialdried over sodium sulfate
7. customPurified
8. customafter removal of the solvent under the reduced pressure
9. washby column chromatography (silica gel, eluted with dichloromethane)