反应详情

In a 5-liter three-necked round bottomed flask was placed 93 g of 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride and 885 mL of water. To the resulting solution were added 138.6 g of sodium bicarbonate followed by 500 mL of ethyl acetate. To the resulting well-stirred mixture was added 123.5 g of 4-amino-3-chloro-5-methoxyiminomethylbenzoyl chloride dissolved in 1000 mL of ethyl acetate at room temperature over a period of 50 minutes. After the addition was complete the reaction mixture was stirred at room temperature for 1 hour. The two phases were separated and the organic layer was washed with water (2×500 mL), brine (1×500 mL), dried over anhydrous magnesium sulfate and the solvent eliminated in a rotary evaporator yielding the crude product as a brown oil. This oil was passed through a short silica gel column using methylene chloride as elution solvent. Evaporation of the solvent yielded 133.3 g of the expected 4-amino-3-chloro-5-methoxyiminomethyl-N-(3-chloro-1-ethyl-1-methyl-2-oxopropyl)benzamide as an off-white solid (mp 140-141° C.).

1. customIn a 5-liter three-necked round bottomed flask was placed
2. additionAfter the addition
3. stirringwas stirred at room temperature for 1 hour
4. customThe two phases were separated
5. washthe organic layer was washed with water (2×500 mL), brine (1×500 mL)
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent eliminated in a rotary evaporator
8. customyielding the crude product as a brown oil
9. washas elution solvent
10. customEvaporation of the solvent