94561-99-6Relevant academic research and scientific papers
Continuous preparation method of DL-muscone
-
Paragraph 0046; 0050; 0053; 0054, (2018/07/15)
The invention discloses a continuous preparation method of DL-muscone. The preparation method comprises the following steps: 1) dissolving 2,15-hexadecanedione diketone in an aprotic solvent, then carrying out a continuous reaction in a fixed-bed cyclization reactor for generating a 3-methylcyclopentanone analogue under the action of a cyclization catalyst; 2) carrying out desolvation on the 3-methylcyclopentanone analogue, dissolving the obtained product in a protic solvent, then carrying out a continuous reaction with hydrogen in a fixed-bed hydrogenation reactor under the action of a hydrogenation catalyst to obtain muscone; and 3) carrying out desolvation on the product obtained in the step 2), carrying out continuous chromatographic separation, and carrying out desolvation on the product liquid containing the DL-muscone to obtain the DL-muscone product. The method for preparing the DL-muscone provided by the invention has high process stability and high product yield, continuous production of the DL-muscone can be realized, the production cost is greatly reduced, and the effective capacity of a device is improved.
(E)-3-METHYL-2-CYCLOALKENONE COMPOUND, 3-HALO-3-METHYLCYCLOALKANONE COMPOUND AND METHOD FOR PRODUCING (R)-3-METHYLCYCLOALKANONE COMPOUND
-
Paragraph 0209-0211, (2018/06/29)
PROBLEM TO BE SOLVED: To provide novel (E)-3-methyl-2-cycloalkenone compounds and 3-halo-3-methylcycloalkanone compounds, and also provide a production method that can efficiently produce (R)-3-methylcycloalkanone compounds. SOLUTION: An (E)-3-methyl-2-cycloalkenone compound has a chemical structure represented by the following formula (1) (where n is an integer of 1-5, 7 or 8). SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
METHOD FOR PRODUCING 3-METHYL CYCLOPENTADECENONES
-
Paragraph 0047-0051, (2017/12/01)
PROBLEM TO BE SOLVED: To provide a method for producing 3-methyl cyclopentadecenones in which the 3-methyl cyclopentadecenones can efficiently be produced. SOLUTION: The 3-methylcyclopentadecenones is produced by an intramolecular condensation reaction of 2,15-hexadecanedione represented by the chemical formula of CH3CO(CH2)12 COCH3. And, in the intramolecular condensation reaction, by using a catalyst having a BET specific surface area of 10 m2/g or less, a decrease in yield due to an increase of the intermolecular condensation reaction on the catalyst can be suppressed as well as, because the deterioration of catalyst can be suppressed, 3-methylcyclopentadecenones can efficiently be produced by the intramolecular condensation reaction. Further, the catalyst is preferably at least one of magnesium oxide, calcium oxide and zinc oxide. SELECTED DRAWING: None COPYRIGHT: (C)2017,JPOandINPIT
A practical synthesis of (rac)-muscone and (R)-(-)-muscone
Cheng, Chuanjie,Ding, Wei,Ding, Shaomin
experimental part, p. 195 - 197 (2011/07/30)
A practical synthesis of (rac)-muscone in three steps is described, using commercially available 1,10-dibromodecane as the starting material. In the first step, an aldol reaction of 1,10-dibromodecane with ethyl acetoacetate affords the important intermediate 2,15-hexadecanedione in 70% yield. A cyclisation reaction in the second step aided by propyl zinc iodide gives dehydro-muscone in 84% yield. Hydrogenation of dehydro-muscone with Pd-C completes the synthesis of (rac)-muscone. Furthermore, (R)-(-)-muscone is enantioselectively prepared via the formation of a ketal intermediate from dehydro-muscone and 1,4-di-O-benzyl-D-threitol.
