HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136354627, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | Ethyl 2-cyano-2-(hydroxyimino)acetate | HCID 6399078 | — |
| Reactant | HCID 21504418 | HCID 21504418 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136354627 | HCID 136354627 | 19.7% |
Reaction Steps
Ethyl α-oximinocyanoacetate (21 g.) was added to a solution of sodium (11.3 g.) in anhydrous methanol (300 ml.). Crude 3,5-dichloro-2-methoxybenzamidine (24 g.) dissolved in a little anhydrous methanol was added, and the mixture was heated to reflux with stirring for 8 hours. The mixture was poured into water (2000 ml.) and acidified with glacial acetic acid. The solid obtained was filtered off, washed with water and recrystallised from glacial acetic acid to give 4-amino-2-(3,5-dichloro-2-methoxyphenyl)-5-nitrosopyrimid-6-one (6.8 g.), m.p. 265° C. (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03987160 |
| Source dataset | uspto-grants-1976_10 |
| ORD ID | ord-2a9a00fc34294efa8386a147bc3deb31 |
| Source note | uspto-grants-1976_10 |