HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → 2-Methylsulfinyl-4-difluoromethoxy-6-methylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | 2-Methylthio-4-difluoromethoxy-6-methylpyrimidine | HCID 694382 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Methylsulfinyl-4-difluoromethoxy-6-methylpyrimidine | HCID 13491826 | 97.2% |
Reaction Steps
A suspension of 20.6 g (0.1 mol) of 3-chloroperoxybenzoic acid in 100 ml of methylene chloride is cooled to a temperature of between -15° C. and -20° C., and there is then added dropwise a solution of 20.6 g (0.1 mol) of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine in 50 ml of methylene chloride. After the reaction mixture has been stirred for 1 hour at the same temperature, it is diluted with methylene chloride; it is subsequently washed with a sodium hydrogen carbonate solution and water, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the residue from a methylene chloride/petroleum ether mixture yields 21.6 g (97% of theory) of 2-methylsulfinyl-4-difluoromethoxy-6-methylpyrimidine, m.p. 105°-107° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04542216 |
| Source dataset | uspto-grants-1985_09 |
| ORD ID | ord-91e088f261b74cc59606b13ba1fa2f35 |
| Source note | uspto-grants-1985_09 |