Calcium Carbonate → HCID 54307017, compound

HRID 1577001Notes

Reaction equation

HRID 1577001 reaction equation
Br[CH2:2][CH:3]=[C:4]([CH3:12])[CH2:5][CH2:6][C:7]([CH3:11])=[C:8]([CH3:10])[CH3:9].[CH2:13]1[O:21][C:20]2[CH:19]=[CH:18][C:17]([OH:22])=[CH:16][C:15]=2[O:14]1.C(=O)([O-])[O-].[Ca+2]>CC(C)=O>[CH3:12][C:4]([CH2:5][CH2:6][C:7]([CH3:11])=[C:8]([CH3:10])[CH3:9])=[CH:3][CH2:2][O:22][C:17]1[CH:18]=[CH:19][C:20]2[O:21][CH2:13][O:14][C:15]=2[CH:16]=1

Participants

5

Reactant 3

HCID 10112Calcium CarbonateHCID 68289SesamolHCID 544893181-Bromo-3,6,7-trimethylocta-2,6-diene

Product 1

HCID 54307017HCID 54307017, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

26 g of 1-bromo-3,6,7-trimethyl-2,6-octadiene, 13 g of 3,4-methylenedioxy-phenol [sesamol] and 20.75 g of finely pulverized calcium carbonate were refluxed for 68 hours in 100 ml of acetone. After reflux the reaction mixture was filtered and the acetone solution was evaporated. By chromatography on Kieselgel with hexane-diethylether (4:1 parts by volume) and distillation under vacuum there was obtained pure 3,6,7-trimethyl-1-[3,4-(methylenedioxy)-phenoxy]-2,6-octadiene, b.p. 114°-117°C/0.002 mmHg; nD20 = 1.5352.

Workup

  1. temperatureAfter reflux the reaction mixture
  2. filtrationwas filtered
  3. customthe acetone solution was evaporated
  4. distillationBy chromatography on Kieselgel with hexane-diethylether (4:1 parts by volume) and distillation under vacuum there

Sources & evidence

ORD record
ord-865a44c208324492a251a70ef9e5ebb2
Source dataset
uspto-grants-1976_09
Patent number
US03983243

Reaction notes

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