HCID 54514636, 화합물 → 3,7,11-Trimethyl-1-dodecene

In 300 ml of hexane were dissolved 50 g of 3,7,11-trimethyl-1-dodecen-3-ol and 0.87 g of pyridine, and 30.8 g of phosphorus tribromide was added dropwise to the solution at 0° to -10° C. After 2 hours of stirring at 0° C., the reaction mixture was poured into water and extracted with hexane. The hexane layer was successively washed with aqueous sodium hydrogen carbonate and aqueous sodium chloride and dried over anhydrous magnesium sulfate. The solvent was distilled off to give 62.5 g of crude 1-bromo-3,7,11-trimethyl-2-dodecene. To a suspension of 14.2 g of zinc in 26 ml of acetic acid was added dropwise 62.5 g of the crude 1-bromo-3,7,11-trimethyl- 2-dodecene and the mixture was stirred at room temperature for 1 hour. Thereafter, the zinc was filtered off and the filtrate was poured into water and extracted with hexane. The hexane layer was washed with aqueous sodium hydrogen carbonate and aqueous sodium chloride in that order and dried over anhydrous sodium sulfate. The solvent was then distilled off and the residue was further distilled under reduced pressure to give 10.6 g (yield 25%) of 3,7,11-trimethyl-1-dodecene. The physical constants of the compound are as follows.

1. filtrationThereafter, the zinc was filtered off
2. additionthe filtrate was poured into water
3. extractionextracted with hexane
4. washThe hexane layer was washed with aqueous sodium hydrogen carbonate and aqueous sodium chloride in that order
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was then distilled off
7. distillationthe residue was further distilled under reduced pressure

ORD 기록

ord-70c283307eeb43d0b8f26df36d8f0ea4

출처 데이터셋

uspto-grants-1990_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04946857