Reaktionsgleichung
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH2:11]([O:13][CH:14]([O:17][CH2:18][CH3:19])[CH:15]=[CH2:16])[CH3:12].C(O)(=O)C>C(#N)C>[CH2:11]([O:13][CH:14]([O:17][CH2:18][CH3:19])[CH2:15][CH2:16][SH:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:2]1[CH3:1])[CH3:12]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
1-(3,3-Diethoxypropyl)-2-methyl-benzothiazole was prepared by reaction of 2-methylbenzothiazole (125 mg, 0.84 mmol) with acrolein diethyl acetal (1.64 g, 12.6 mmol) and acetic acid (100 μl) in acetonitrile (4 ml) by a method analogous to that described in Section 1.2. The product was purified by HPLC on a Rainin Dynamax C18, 8 μm using a 0-100% gradient elution of water/acetonitrile (containing 0.1% TFA) over 60 minutes at 20 ml/min. The product was obtained as a colourless oil (220 mg, 95%); m/z (FAB+): 280.
Aufarbeitung
- customThe product was purified by HPLC on a Rainin Dynamax C18, 8 μm
- washa 0-100% gradient elution of water/acetonitrile (containing 0.1% TFA) over 60 minutes at 20 ml/min
Quellen und Nachweise
- ORD-Eintrag
- ord-7eb7199aec9b47b9bd24813aa90a4f74
- Quelldatensatz
- uspto-grants-2000_10
- Patentnummer
- US06133445
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