Reaktionsgleichung
Br[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:5]=2[N:6]=1.ClC1S[C:15]2[CH:21]=CC=C(Cl)[C:16]=2N=1.[OH-:23].[Na+].O>C(O)CC>[CH2:21]([O:23][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:5]=2[N:6]=1)[CH2:15][CH3:16]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A mixture (11.30 g, 0.05 mole) of 2-bromo-4-chlorobenzothiazole and 2,4-dichlorobenzothiazole and 94% sodium hydroxide (2.34 g, 0.055 mole) in n-propanol (100 c.c.) was heated under reflux for 1 hour. Water was added and the alcohol was distilled azeotropically together with water. The resulting oily substance was extracted with chloroform, and the chloroform layer was washed with water. The solvent was removed under reduced pressure to obtain 11.12 g of 2-n-propoxy-4-chlorobenzothiazole as a yellow viscous liquid. Yield 97.7%, purity 98.9%, b.p. 106°-108° C./0.12 mmHg.
Aufarbeitung
- temperatureunder reflux for 1 hour
- distillationthe alcohol was distilled azeotropically together with water
- extractionThe resulting oily substance was extracted with chloroform
- washthe chloroform layer was washed with water
- customThe solvent was removed under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-705986d35b744ee8a86accc645a337d5
- Quelldatensatz
- uspto-grants-1981_10
- Patentnummer
- US04293702
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