7-METHOXY-1-METHYL-2-TETRALONE synthesis
- Product Name:7-METHOXY-1-METHYL-2-TETRALONE
- CAS Number:1204-23-5
- Molecular formula:C12H14O2
- Molecular Weight:190.24
4133-34-0
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1204-23-5
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Yield: 85%
Reaction Conditions:
with N-ethyl-N,N-diisopropylamine in dichloromethane at 0 - 20; for 4.33 h;
Steps:
1 Preparation of methylated product II
7-Methoxy-2-tetralone I (17.6 g, 0.10 mol) was dissolved in 30 ml of dichloromethane,The reaction was cooled to 0 ° C,N, N-diisopropylethylamine (13.6 ml, 0.1 mol) was added portionwise to the reaction system,At this temperature,Slowly add cooled methyl iodide (6.22 ml, 0.1 mol)Dropping time more than 20 minutes.After the addition was complete, the temperature was naturally warmed to room temperature, and reacted at room temperature for 4 hours.TLC point plate, the basic point of disappearance of raw materials. Then adjust the pH to neutral with saturated ammonium chloride solution,Followed by three extractions with EtOAc, each time using 25 ml.The combined organic phases were washed with saturated sodium chloride, dried over magnesium sulfate,Concentration and column chromatography gave 16.2 g of methylated product II in 85% yield.
References:
Wenzhou Medical University;Feng Jianpeng;Liang Guang;Liu Zhiguo;Zhang Yali;Cai Yuepiao;Lu Kongqin CN104910002, 2017, B Location in patent:Paragraph 0019-0020; 0022-0023
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