3′,4′-(Methylenedioxy)propiophenone synthesis
- Product Name:3′,4′-(Methylenedioxy)propiophenone
- CAS Number:28281-49-4
- Molecular formula:C10H10O3
- Molecular Weight:178.18
Yield:28281-49-4 311 g
Reaction Conditions:
with zinc(II) oxide;zinc(II) chloride in dichloromethane at 0 - 5; for 5 h;Reagent/catalyst;Solvent;
Steps:
1-6 Preparation of dihydrosafrole (using 0.5 moles of Zinc oxide and 0.05 moles of Zinc chloride per mole of acyl chloride using dichloromethane as solvent)
488 g of 1,3-benzodioxole and 750 g of dichloromethane were charged into a 3 liter reaction flask and the mixture was cooled to 0°C under stirring. 162 g of Zinc oxide and 27 g of Zinc chloride were added under stirring at 0°C. Subsequently, 370 g of propionyl chloride was added to the above mixture in 4 hours, maintaining the temperature of the reaction medium between 0°C and 5°C under stirring. The reaction medium was stirred for another 1 hour till the acylation reaction was substantially completed. The reaction mass was subjected to aqueous workup to remove Zinc chloride and propionic acid and the organic layer was separated and distilled to recover 245 g of unreacted 1,3-benzodioxole, and 311 g of methylenedioxybenzene propiophenone with a GC purity of >99%. The methylenedioxybenzene propiophenone was subjected to selective reduction and dehydration as discussed in Example 1 to obtain 271 g of dihydrosafrole with a yield of 111.5% (wt./wt. on 1,3-benzodioxole consumed) and purity of > 99% by GC analysis.
References:
WO2018/150230,2018,A1 Location in patent:Paragraph 0065-0076
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