反应详情

温度

80 °C

Paraformaldehyde (600 mg) and a 50% aqueous dimethylamine solution (1.80 g) were added to a solution of tert-butyl {(3R)-1-[5-(2-chlorobenzyl)-1,3-dimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-pyrrolo[3,2-d]pyrimidin-6-yl]piperidin-3-yl}carbamate (1.00 g) in a mixture of ethanol (10 ml) and acetic acid (5 ml), and the resulting mixture was stirred with heating at 80° C. After the reaction solution was cooled to 25° C., toluene (30 ml) was added thereto and the resulting mixture was concentrated under reduced pressure. This procedure was repeated three times. The resulting residue was acidified with a 10% aqueous potassium hydrogensulfate solution and extracted twice with chloroform (100 ml). The organic layer was dried over sodium sulfate and filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by a silica gel column chromatography (hexane/ethyl acetate=1/2) to obtain the title compound (913 mg).

1. temperatureAfter the reaction solution was cooled to 25° C.
2. concentrationthe resulting mixture was concentrated under reduced pressure
3. extractionextracted twice with chloroform (100 ml)
4. dry with materialThe organic layer was dried over sodium sulfate
5. filtrationfiltered
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe resulting residue was purified by a silica gel column chromatography (hexane/ethyl acetate=1/2)