pyrrolizidine-7α-acetic acid methyl ester synthesis
- Product Name:pyrrolizidine-7α-acetic acid methyl ester
- CAS Number:78449-76-0
- Molecular formula:C10H17NO2
- Molecular Weight:183.25
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Yield:78449-76-0 40.8%
Reaction Conditions:
at 80 - 145; for 14 h;Temperature;
Steps:
9-11 Preparation of 7α-bis-pyrrolidin-methyl acetate (VIII)
Add 50 g of monomethyl malonate, 37.02 g (0.28 mol) of N-(3-carboxypropyl)butyrolactam (III) to a 500 mL four-necked flask equipped with a mechanical stirring and a thermometer, and raise the temperature to 140-145 ° C. , stirring for 2 hours, cooling to 80-85 ° C, adding 51.5 g (0.33 mol) of human malonate monomethyl ester potassium salt dissolved in 300 ml of monomethyl malonate solution, stirring for 12 hours, cooling to room temperature, Adding to 500 ml of water, adjusting to pH=10-11 with sodium hydroxide, extracting with dichloromethane (100 ml×3), combining the organic phases, and drying and concentrating to obtain a colorless liquid 7α-bis-pyrrolidine-methyl acetate ( VIII) 16.2 g, yield 40.8%.
References:
CN109867679,2019,A Location in patent:Paragraph 0068-0077
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