HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178502002, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | HCID 178502003 | HCID 178502003 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178502002 | HCID 178502002 | — |
Reaction Steps
3.5 g of crude methyl 2-amino-6-[(p-tolylsulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide are dissolved in 100 ml of methylene chloride and 50 ml of tetrahydrofuran. At 0° there are added thereto 2.2 g of N-methylmorpholine and subsequently 1.45 ml of methyl chloroformate in 20 ml of methylene chloride. The mixture is stirred at 0° for 1 hour and then at room temperature for 2 hours and thereupon treated with a small amount of methanol and water. The organic phase is separated, dried and evaporated. The residue is recrystallized from methylene chloride and ether, there being obtained pure dimethyl 6-[(p-tolylsulfonyl)oxy]-2,4-pyrimidinedicarbamate-3-oxide of melting point 178°-179°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04549019 |
| Source dataset | uspto-grants-1985_10 |
| ORD ID | ord-149eb55cdee540ceb1a328498b1e4da1 |
| Source note | uspto-grants-1985_10 |