Sodium Chloride → tert-Butyl 2-(3,4-dichloro-N-methylphenylsulfonamido)-4,5,6,7-tetrahydrobenzo-[b]thiophene-3-carboxylate
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([NH:12][C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[C:29]([O-])([O-])=O.[K+].[K+].CI.[Na+].[Cl-]>CC(C)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]([C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH3:29])(=[O:10])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
tert-Butyl 2-(3,4-dichlorophenylsulfonamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate (21.64 g, 46.8 mmol) was dissolved in acetone (200 ml), and K2CO3 (12.9 g, 93.6 mmol) was added thereto. Methyl iodide (5.83 ml, 93.6 mmol) was then added, and the suspension was heated overnight at 40° C. After cooling to room temperature, water and saturated NaCl solution were added and the product was extracted with ethyl acetate. The organic phase was dried (sodium sulfate) and the product was purified by crystallization from methanol.
Aufarbeitung
- temperatureAfter cooling to room temperature
- extractionthe product was extracted with ethyl acetate
- dry with materialThe organic phase was dried (sodium sulfate)
- customthe product was purified by crystallization from methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-9ad16240addf439ea3b53b7601ff98fa
- Quelldatensatz
- uspto-grants-2012_02
- Patentnummer
- US08119633B2
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