HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 13961960, compound → HCID 178503558, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 13961960 | HCID 13961960 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178503558 | HCID 178503558 | 70.8% |
Reaction Steps
Over 50 minutes, a solution of 8.8 g (0.127 mole) of sodium nitrite in 10 ml of dimethylformamide is added dropwise at 140° C. to a solution of 8.7 g (0.038 mole) of 4-chloro-6-difluoromethoxy-2-methylthiopyrimidine in 10 ml of dimethylformamide. When the addition of the sodium nitrite is complete, the mixture is stirred for 2 hours at 140° to 150° C. The solvent is then evaporated off in vacuo and the residue is crystallised from 1N hydrochloric acid, affording 5.6 g (70% of theory) of 4-difluoromethoxy-6-hydroxy-2-methylthiopyrimidine with a melting point of 236°-237° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04692524 |
| Source dataset | uspto-grants-1987_09 |
| ORD ID | ord-d2b6cc7673524f8a89b8382c16ec5160 |
| Source note | uspto-grants-1987_09 |