6-Ethylthio-3-hepten-2-one synthesis
- Product Name:6-Ethylthio-3-hepten-2-one
- CAS Number:81008-52-8
- Molecular formula:C9H16OS
- Molecular Weight:172.29
3916-64-1
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Yield:81008-52-8 1011 g
Reaction Conditions:
Stage #1: hepta-3,5-dien-2-onewith triethylamine at 20 - 25; for 0.25 h;Large scale;
Stage #2: ethanethiol at 55 - 65;Large scale;
Steps:
1 preparation of 6-ethylthio-3-hepten-2-one
To the reaction flask was added 100 g (purity 97.8 , 0.888 mol) of 3,5-heptadien-2-one (Formula II), 2.76 g (0.027 mol) of triethylamine at room temperature (20-25 ° C) After stirring for 15 minutes, slowly raise to 55 ° C and start dropping 60.69 g (0.977πο1) ethanethiol. The dropping temperature was controlled at 55-65 ° C. After dripping, the temperature was maintained at 55-65 ° C The reaction was complete for 3 hours, and the gas chromatographic tracking reaction was complete (3,5-heptadien-2-one) at room temperature (20-25 ° C), and 400 ml of water and 1000 ml of toluene were added and stirred for 30 minutes. 30 minutes,The organic layer and then add 200ml of water to stir for 30 minutes, put it aside for 30 minutes, separated, toluene layer of pressure to return to the water, the separation of the organic layer, add 100ml of 0.5% dilute hydrochloric acid, stirring and washing, When the water content of the reaction solution was <0.1%, the water was allowed to cool to room temperature to obtain 1011 g of a 6-ethylthio-3-heptene-2-ketone /Gas purity (deduction of toluene solvent peak) 97.1% After the purification of 0.820mol, the molar yield of 92.34%.
References:
CN107162945,2017,A Location in patent:Paragraph 0064; 0070; 0071
