HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 2-Methylamino-4-difluoromethoxy-6-methylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 2-Methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine | HCID 13491821 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Methylamino-4-difluoromethoxy-6-methylpyrimidine | HCID 13491822 | 74% |
Reaction Steps
30 ml of a 40% aqueous methylamine solution are added, at a temperature of between 20° and 25° C., to 2.2 g (0.009 mol) of 2-methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine. The mixture warms up to a temperature of 60° C. The reaction mixture is subsequently stirred for half an hour at the same temperature; it is then cooled and 50 ml of methylene chloride are added. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the residue from a methylene chloride/petroleum ether mixture yields 1.4 g (74% of theory) of 2-methylamino-4-difluoromethoxy-6 -methylpyrimidine, m.p. 129.5°-131° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04542216 |
| Source dataset | uspto-grants-1985_09 |
| ORD ID | ord-4edbee7928b040dba5cfc47cfc7e2dee |
| Source note | uspto-grants-1985_09 |