HCID 21461387, compound → HCID 15788050, compound

Participants

Reaction Steps

0.943 mol (105.8 g) of potassium tert.butylate were dissolved in 800 ml of water-free THF. A solution of 865 mmol (231 g) of 4-bromomethyl-9,9-dimethyl-3,5,8,10-tetraoxabicyclo[5.3.0]decane in 800 ml of THF were added dropwise within 90 minutes with stirring and the mixture was subsequently heated for 6 h under reflux. The resulting KBr was filtered and the THF was subsequently distilled under a filter pump vacuum. The dark brown residue underwent fractional distillation under vacuum. 111.2 g of colourless clear 4-methylene-9,9-dimethyl-3,5,8,10-tetraoxabicyclo[5.3.0]decane (yield 70%) go over at between 45° and 49° C. (0.2 mbar).

Provenance & Evidence