反应详情

温度

5 °C

A mixture of the solution of Step B and 6 ml of triethylamine was refluxed for 3 hours and was then cooled and poured into 2 N aqueous hydrochloric acid. The decanted organic phase was washed with water, dried and evaporated to dryness. The residue was taken up in 20 ml of hot methylene chloride and after the addition of 30 ml of n-heptane thereto, the mixture was cooled to 5° C. and vacuum filtered. The recovered product was washed with heptane and dried to obtain 3.025 g of (1R,3S) 3-[(dihydro-2-oxo-3(2H)-thienylidene)-methyl]-2,2-dimethyl-cyclopropane-1-carboxylic acid melting at 162° C.

1. temperaturewas refluxed for 3 hours
2. temperaturewas then cooled
3. washThe decanted organic phase was washed with water
4. customdried
5. customevaporated to dryness
6. additionafter the addition of 30 ml of n-heptane
7. filtrationvacuum filtered
8. washThe recovered product was washed with heptane
9. customdried