3,7,11,15-TETRAMETHYL-2-HEXADECEN-1-OL synthesis
- Product Name:3,7,11,15-TETRAMETHYL-2-HEXADECEN-1-OL
- CAS Number:7541-49-3
- Molecular formula:C20H40O
- Molecular Weight:296.53
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Yield:7541-49-3 89%
Reaction Conditions:
Stage #1: isophytolwith phosphorus tribromide in n-heptane at -10 - 0; for 1 h;
Stage #2: with sodium hydroxide in water at 50 - 60; pH=6 - 7; for 2 h;
Steps:
9 Example 9 Phytoalcohol
Add n-heptane 300 to the reaction flask ml, isophytoalcohol 80g (0.27mol), lower the temperature to below 0°C, add 32g (0.12mol) phosphorus tribromide dropwise, and stir for 1 hour at -100°C. After the reaction is completed, add 30g water dropwise below 10°C Add 150ml of water, 10% sodium hydroxide to adjust the pH to 6~7, then add a solution consisting of 30g of sodium hydroxide and 30g of water, stir and react at 50~60 for 2 hours, adjust the pH to 6~7 with hydrochloric acid, and let stand Separate the layers, wash the organic layer with water, dry with anhydrous sodium sulfate, and recover the n-heptane under reduced pressure to obtain crude plant alcohol oil. The crude oil was rectified, and the 2mmHg 160170 fraction was collected to obtain 65g of light yellow oily liquid of plant alcohol with a yield of 81%, or the crude oil was chromatographed on silica gel column to determine the n-heptane: ethyl acetate (volume ratio) 10:1) is the eluent to obtain 71 g of light yellow oily liquid of plant alcohol, with a yield of 89%
References:
CN111393275,2020,A Location in patent:Paragraph 0061; 0100-0101
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