反应详情

To a mixture of 5.02 g (0.025 mole) of 3-cyclopentylamino-2,2-dimethyl-propanoic acid methyl ester, 5.30 g (0.0276 mole) of 2,4-dichloro-5-nitro-pyrimidine and 100 mL of ether was added 20 mL of water and 5.00 g (0.050 mole) of potassium bicarbonate. The mixture was stirred at room temperature for 14 hours. The resulting two-layer mixture was separated and the aqueous layer was extracted twice with 20 mL of ether. The combined ether extracts were washed successively with 20 mL of aqueous sodium carbonate, twice with 20 mL of brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 8.60 g of 3-[(2-chloro-5-nitro-pyrimidin-4-yl)-cyclopentyl-amino]-2,2-dimethyl-propanoic acid methyl ester (IV-38) as a yellow solid.

1. customThe resulting two-layer mixture was separated
2. extractionthe aqueous layer was extracted twice with 20 mL of ether
3. washThe combined ether extracts were washed successively with 20 mL of aqueous sodium carbonate, twice with 20 mL of brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure