HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Isocyanate → HCID 54387530, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Isocyanate | HCID 12228 | — |
| Reactant | 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime | HCID 136352416 | — |
| Catalyst | Di-n-butyl diacetoxy tin | HCID 9798523 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54387530 | HCID 54387530 | 71.2% |
Reaction Steps
A mixture of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime (1.5 g), methyl isocyanate (0.705 g), and dibutyltin diacetate (2 drops) was stirred in dichloromethane at 20° C. in a sealed bottle for 2 days. The mixture was partitioned between water and dichloromethane, the organic layer dried (Na2SO4) and evaporated and the residue crystallized from ethyl acetate/hexane to give 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde O-(N-methylcarbamoyl)oxime (1.22 g) m.p.146-147° C. Compound 18.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06638956B2 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-6c8d6e7aadb845f79974c931c71e91a8 |
| Source note | uspto-grants-2003_10 |