Methyl Isocyanate → 3'-Chloro-4'-(N-methylcarbamoyloxy)-5'-nitroacetophenone
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([C:12](=[O:14])[CH3:13])[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[OH:8].[CH3:15][N:16]=[C:17]=[O:18]>>[Cl:1][C:2]1[CH:3]=[C:4]([C:12](=[O:14])[CH3:13])[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[O:8][C:17](=[O:18])[NH:16][CH3:15]Komponenten
3
Versuchsvorschrift
A mixture of 21.5 grams (0.1 mole) 3'-chloro-4'-hydroxy-5'-nitroacetophenone and 85.0 milliliters (a large excess) of methylisocyanate was refluxed for 5 hours. On cooling, a white crystalline product was formed. The product was filtered (weight 18.0 grams, melting point 115°-118° C.) and was identified by characteristic peaks in the infrared spectrum as 3'-chloro-4'-(N-methylcarbamoyloxy)-5'-nitroacetophenone.
Aufarbeitung
- temperaturewas refluxed for 5 hours
- temperatureOn cooling
- customa white crystalline product was formed
- filtrationThe product was filtered (weight 18.0 grams, melting point 115°-118° C.)
Quellen und Nachweise
- ORD-Eintrag
- ord-2d1d34664ce748c9befeff1e2ea8202e
- Quelldatensatz
- uspto-grants-1976_01
- Patentnummer
- US03933472
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