Sodium Carbonate → HCID 2859367, compound

Participants

Reaction Conditions

Reaction Steps

A 3,000 mL, 3-necked, round-bottom flask was equipped with a mechanical stirrer, a reflux condenser and a 250 mL addition funnel. The flask was charged with H2O (1,500 mL) and 70% HClO4 (1 mL) and heated to ca. 80° C. while stirring vigorously (ca. 750 rpm). 4-Allyl-2-methoxyphenyl glycidyl ether was placed in the addition funnel and was added dropwise to the reaction mixture over a 4-5 hour period. The reaction mixture was stirred for 48 hours at ca. 80° C. The mixture was then allowed to cool and was neutralized with 5% Na2CO3. The phases were separated and the aqueous phase extracted with CH2Cl2 (1,500 mL). The CH2Cl2 and H2 were removed from the 3-(4-allyl-2-methoxyphenoxy)-1,2-propanediol, i.e., ##STR23## by evaporation in vacuo to yield a pale amber oil (355 g, 97%) which crystallized on standing; mp 77°-79° C. (recrystallized from benzend).

Provenance & Evidence