Reaktionsgleichung
[C:1](Cl)(=[O:9])[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)([O-])O.[Na+].O.[NH2:17][C:18]1[S:19][C:20]2[CH:26]=[C:25]([S:27][C:28]#[N:29])[CH:24]=[CH:23][C:21]=2[N:22]=1>O1CCCC1>[S:27]([C:25]1[CH:24]=[CH:23][C:21]2[N:22]=[C:18]([NH:17][C:1](=[O:9])[O:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[S:19][C:20]=2[CH:26]=1)[C:28]#[N:29]Komponenten
Reaktionsbedingungen
- Temperatur
- 20 °C
Versuchsvorschrift
7.5 g of phenyl chlorocarbonate and then 4.05 g of sodium hydrogen carbonate and 9.4 cm3 of water are added, at 20° C., to a solution of 2.5 g of commercial 2-amino-1,3-benzothiazol-6-yl thiocyanate in 94 cm3 of tetrahydrofuran. The resulting mixture is subsequently stirred at 20° C. for 20 h and then extracted with 2×150 cm3 of ethyl acetate. The organic phases are combined and then washed with 3×50 cm3 of a saturated aqueous solution of sodium hydrogen carbonate. The organic phase obtained is dried over magnesium sulphate and then concentrated to dryness under reduced pressure. The residue is taken up in 50 cm3 of water and the product is spin-filter-dried and dried under vacuum at 20° C. 3.45 g of phenyl (6-thiocyanato-1,3-benzothiazol-2-yl)carbamate are thus obtained in the form of a pale yellow solid, the characteristics of which are as follows:
Aufarbeitung
- extractionextracted with 2×150 cm3 of ethyl acetate
- washwashed with 3×50 cm3 of a saturated aqueous solution of sodium hydrogen carbonate
- customThe organic phase obtained
- dry with materialis dried over magnesium sulphate
- concentrationconcentrated to dryness under reduced pressure
- customthe product is spin-filter-dried
- customdried under vacuum at 20° C
Quellen und Nachweise
- ORD-Eintrag
- ord-c93db23857eb44e8ada5e57a595711e9
- Quelldatensatz
- uspto-grants-2013_10
- Patentnummer
- US08546393B2
Verknüpfte Notizen
Wird geladen…