Dithiocarbonic acid O-tert-butyl ester S-methyl ester synthesis
- Product Name:Dithiocarbonic acid O-tert-butyl ester S-methyl ester
- CAS Number:37527-08-5
- Molecular formula:C6H12OS2
- Molecular Weight:164.29
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Yield:37527-08-5 60%
Reaction Conditions:
Stage #1: carbon disulfide;potassium-t-butoxide in 5,5-dimethyl-1,3-cyclohexadiene at 80; for 1 h;
Stage #2: methyl iodine in 5,5-dimethyl-1,3-cyclohexadiene;diethyl ether at 20; for 20 h;
Steps:
Methyl O-(tert-butyl)S-dithiocarbonate
Potassium tert-butoxide (73.7g, 0.66mol) was added to xylene (2L), the temperature was raised to 80°C, carbon disulfide (50g, 0.66mol) was added dropwise, the reaction was carried out at 80°C for 1 h, cooled to room temperature, filtered, and ether Washed and dried to obtain 100 g of light yellow solid. The solid was added to ether (1 L), methyl iodide (113 g, 0.796 mol) was added, the reaction was carried out at room temperature for 20 h, filtered, the solid was washed with ether, and the filtrate was concentrated under reduced pressure to obtain the title compound INT- 3B (65g, 60%).
References:
WO2022/135390,2022,A1 Location in patent:Page/Page column 40
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