Sodium Iodide → HCID 20320776, Verbindung

1-Chloro-3-(spiro[3.3]hept-2-yl)-1E-propen-3-one (7.3 g, 0.042 mole) was mixed with 25.2 g (0.168 mole) of sodium iodide and 45 ml of dry acetone (distilled from anhydrous potassium carbonate, b.p. 56° C). The mixture was refluxed with rapid stirring overnight. The mixture was cooled and the solvent was removed in vacuo. The solid residue was taken up in 75 ml of water and the products were extracted with 150 ml (3×50 ml) of ether. The organic material was washed with 50 ml of saturated sodium bicarbonate solution, 50 ml of aqueous sodium thiosulfate solution and 50 ml of saturated sodium chloride solution. The material was dried over anhydrous magnesium sulfate, filtered and the solvent was removed in vacuo to yield 6.9 g (62.2%) of crude 1-iodo-3-(spiro[3.3]hept-2-yl)-1E-propen-3-one.

1. temperatureThe mixture was refluxed
2. temperatureThe mixture was cooled
3. customthe solvent was removed in vacuo
4. extractionthe products were extracted with 150 ml (3×50 ml) of ether
5. washThe organic material was washed with 50 ml of saturated sodium bicarbonate solution, 50 ml of aqueous sodium thiosulfate solution and 50 ml of saturated sodium chloride solution
6. dry with materialThe material was dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customthe solvent was removed in vacuo

ORD-Eintrag

ord-f0b7d444b87a476792deff1346e53b79

Quelldatensatz

uspto-grants-1978_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04098823