Reaktionsgleichung
[C:1]([C:3]1[N:4]=[CH:5][S:6][CH:7]=1)#[N:2].Cl.[C:9]1(N)[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH2:15]>>[CH:13]1[CH:14]=[CH:9][C:10]2[N:15]=[C:1]([C:3]3[N:4]=[CH:5][S:6][CH:7]=3)[NH:2][C:11]=2[CH:12]=1Komponenten
Reaktionsbedingungen
- Temperatur
- 201 °C
Versuchsvorschrift
The mixture was heated and when the pot temperature reached 164° C., distillation commenced. The temperature gradually increased to 201° C. and a total of 44 ml of water plus ethylene glycol distillate were removed. The mixture was allowed to cool to 100° C. before 27.5 g (0.25 moles) of 4-cyanothiazole were added to the solution containing o-phenylenediamine monohydrochloride. The reaction mixture was heated to 125° C. and held within a temperature range of 125°-130° C. for a period of 5 hours. Thiabendazole formed as a precipitte during the 5 hours of heating. The reaction was monitored by gas chromatography and determined to be complete when the peaks corresponding to o-phenylenediamine and 4-cyanothiazole were negligible. Next, the reaction mass was cooled to 50° C. and filtered to collect the precipitate using a Buchner funnel and #4 Whatman filter paper. The wet cake was washed with 1.5 L of deionized water. The washed precipitate was dried overnight in a vacuum oven under 15-20" Hg and at a temperature of 90° C. The weight of dry thiabendazole crystals was 38.0 g, which corresponds to a yield of 75.5%. The purity was determined to be 99.67% (based on area %) using HPLC analysis.
Aufarbeitung
- temperatureThe mixture was heated
- customreached 164° C.
- distillationdistillation
- customa total of 44 ml of water plus ethylene glycol distillate were removed
- additionwere added to the solution
- temperatureThe reaction mixture was heated to 125° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-ec6ddd42289542fcae7ecc188b583293
- Quelldatensatz
- uspto-grants-1994_05
- Patentnummer
- US05310923
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