METHYL 4,4-DIMETHYL-2-OXOCYCLOHEXANECARBOXYLATE synthesis
- Product Name:METHYL 4,4-DIMETHYL-2-OXOCYCLOHEXANECARBOXYLATE
- CAS Number:32767-46-7
- Molecular formula:C10H16O3
- Molecular Weight:184.23
2979-19-3
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616-38-6
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32767-46-7
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Yield: 92%
Reaction Conditions:
Stage #1:carbonic acid dimethyl ester with sodium hydride in tetrahydrofuranReflux;Inert atmosphere;
Stage #2:3,3-dimethylcyclohexanone in tetrahydrofuran for 4 h;Reflux;
Steps:
1.8 Step 8: 4,4-Dimethyl-2-oxocyclohexanecarboxylic acidMethyl ester
To 15 mL of anhydrous THF was added sodium hydride (1.25 g, 31.3 mmol, 2.0 eq) andDimethyl carbonate (6.5 g,72.0 mmol, 4.6 eq), refluxed under nitrogen, and 8 mL of 3,3-dimethylcyclohexanone (2.0 g,16.0 mmol, 1.0 eq) in THF. The reaction was refluxed for 4 h. To the reaction solution was added 5 mL of methanol, followed by addition of 40 mL of water, DCM (30 mL x 3). The organic phase was dried over anhydrous sodium sulfate, spin-dried, PE / EA (v / v) = 100 / Color liquid product 2.8g, yield 92.0%.
References:
Sunshine Lake Pharma Co.,Ltd.;Kou, Yuhui;Hu, Bolin;Jiang, Haigang;Ye, Jiuyong;Liu, Zhiqiang;Xie, Hongming;Zhang, Yingjun CN106565706, 2017, A Location in patent:Paragraph 0191; 0192; 0193
2979-19-3
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17640-15-2
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32767-46-7
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4694-17-1
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32767-46-7
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1193-18-6
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32767-46-7
35 suppliers
$120.00/50mg