Hydrochloric Acid → HCID 14197812, compound

Participants

Reaction Conditions

Reaction Steps

Under an atmosphere of nitrogen the reaction flask is charged with 9.85 g magnesium and 100 ml diethyl ether. The Grignard reaction is started with 3.00 g bromo-heptane. Then a solution of 70.00 g bromo-heptane in 50 ml diethyl ether is added dropwise within 90 minutes, the reaction mixture is kept at mild reflux and subsequently cooled to 0° C. to add now within 30 minutes a solution of 28.70 g 2-methyl-2-propenal in 30 ml diethyl ether. After further stirring for 2 hours at room temperature the reaction mixture is again cooled to 0° C. and 50 ml of diluted hydrochloric acid (3.5%) are carefully added. The organic layer is washed with water, dried with sodium sulfate and subsequently concentrated to give 86.7 g crude material. Distillation over a 10 cm-column (Widmer type) gives 40.5 g 2-methyl-1-decen-3-ol having a boiling point of 75° C. at 0.12 bar.

Provenance & Evidence