ChemicalBook CAS DataBase List 1-Phenyldecane-1,3-dione

1-Phenyldecane-1,3-dione synthesis

6synthesis methods

Product Name:1-Phenyldecane-1,3-dione
CAS Number:68892-13-7
Molecular formula:C16H22O2
Molecular Weight:246.34

111-11-5 Synthesis

111-11-5
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98-86-2 Synthesis

98-86-2
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68892-13-7
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Yield:68892-13-7 98.3%

Reaction Conditions:

with sodium methylate in 5,5-dimethyl-1,3-cyclohexadiene; for 1.25 h;Inert atmosphere;Reflux;Microwave irradiation;Claisen Condensation;

Steps:

7 EXAMPLE 7Synthesis of OctanoylBenzoylMethane (OBM) usingthe Process According to the Invention

10130] The experimental apparatus consists of a classic glass, double jacketed chemical engineering reactor with a volume of 1 litre with an effective mixing system. This is topped with a separating column fitted with a variable-reflux condenser. It also has a recirculating loop fitted with a geartype pump and a 600 W microwave generatot 10131] Add 550 mE xylenes, 94.78 g fused methyl octanoate and 34.05 g powdered sodium methoxide. Once the reagents have been added, render the reactor inert with a continuous flow of nitrogen gas. Recirculate the mixture through the external circuit at a rate of 15 kg/h. Bring to boiling and total reflux, and then switch the microwave sourceon.10132] Add 68.41 g acetophenone over one hout Once it has all been added, let the reaction continue for another 15 minutes. Throughout all this time, draw the methanol off the reaction mixture. After the 15 minutes of finishing time, switch off the microwave source and the heatet AcidiFy the mixture and then wash it.10133] Analysis of the organic phase by gas phase chromatography shows that almost all the acetophenone is consumed and that the OBM titre is 98.3%. OBM productivity during the reaction phase is 110.3 kg/hIm3.

References:

US2014/88325,2014,A1 Location in patent:Paragraph 0130; 0131; 0132; 0133

638-45-9 Synthesis