3-(4-METHOXY-BENZYLSULFANYL)-3-METHYL-BUTYRIC ACID synthesis
- Product Name:3-(4-METHOXY-BENZYLSULFANYL)-3-METHYL-BUTYRIC ACID
- CAS Number:268219-99-4
- Molecular formula:C13H18O3S
- Molecular Weight:254.35
541-47-9
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6258-60-2
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268219-99-4
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Yield:268219-99-4 338 g
Reaction Conditions:
with piperidine in tetrahydrofuran;hexane at 35 - 80; for 20 h;
Steps:
1 Step 1 : Synthesis of 3-[(4-methoxybenzyl)sulfanyl]-3-methylbutanoic acid
3-Methylbut-2-enoic acid (179 g, 1.78 mol) was added to piperidine (276 g, 3.24 mol), followed by (4-methoxyphenyl)methanethiol (250 g, 1.62 mol) while maintaining the temperature at 35°C. The reaction mixture was heated to 80°C. After 20 hours, t-butyl methyl ether (1.0 L) was added to the mixture, and the reaction mixture was filtered. The residue was partitioned between a biphasic mixture of ethyl acetate (1.5 L) and aqueous hydrochloric acid (1.0 L, 3 M). The organic phase was washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to afford 338 g of the product, which was used directly in the next step without purification. LC-MS m/z 275.9 [M+Na+]; retention time = 0.783 minutes (Method 13).
References:
WO2018/138591,2018,A1 Location in patent:Page/Page column 200
6258-60-2
158 suppliers
$6.00/1g
268219-99-4
14 suppliers
$65.00/100mg
924-50-5
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268219-99-4
14 suppliers
$65.00/100mg