2-Azabicyclo[2.2.1]hept-5-en-3-one synthesis
- Product Name:2-Azabicyclo[2.2.1]hept-5-en-3-one
- CAS Number:49805-30-3
- Molecular formula:C6H7NO
- Molecular Weight:109.13
Yield:49805-30-3 95%
Reaction Conditions:
with sodium hydroxide in methanol at 0 - 5; pH=4 - 5; for 8 h;Diels-Alder Cycloaddition;
Steps:
1 Embodiment 1
In the with of the thermometer and the tail gas absorption device 1000 ml of in [...], adding 500 ml of methanol, 50 g cross-linked polystyrene-sulfinyl and sodium 5.0 g of cyclopentadiene, control low-temperature 0 - 5 °C, slow access 2.5 g cyanogen chloride gas, at the same time dropping 5% of sodium hydroxide in an alcoholic solution, control pH value is 4 - 5 between. The end of the dropping, the reaction to 8 hours. Filtering, separating out the solid.This solid is added to the 100 ml 5% alcoholic solution of acetate, to continue the reaction at room temperature for 8 hours, filtering the solid catalyst particles, the filtrate is concentrated, separating white crystal product, is azabicyclo [2, 2, 1] heptyl -5 - ene -3 - one, the product quality is 4.21 g, yield is 95% (relative to the cyanogen chloride), purity 99.5%.
References:
CN107805217,2018,A Location in patent:Paragraph 0036-0043
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49805-30-3
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