Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| Reactant | 4-Isocyanato-1-nitro-2-(trifluoromethyl)benzene | HCID 15342561 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 20312933 | HCID 20312933 | 44.3% |
Reaction Steps
24 ml of triethylamine were added over 5 minutes to a stirred mixture of 15 g of N-methylhydroxylamine hydrochloride in 100 ml of chloroform cooled to 0° C and then 37.5g of 3-trifluoromethyl-4-nitrophenyl isocyanate were added at 20° to 25° C. The mixture was stirred at 20° C for 16 hours and was then poured into water. The mixture was vacuum filtered and the recovered crystals were dried under reduced pressure. The raw product was taken up in hot isopropyl ether and the solution was treated with activated carbon and was evaporated to dryness under reduced pressure to obtain 20 g of N-hydroxy-N-methyl-N'-(3'-trifluoromethyl-4'-nitrophenyl)-urea melting at 129°-130° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04108993 |
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| Source dataset | uspto-grants-1978_08 |
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| ORD ID | ord-2d4e809a04ef481c902f1e55a57ac474 |
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| Source note | uspto-grants-1978_08 |
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