Reaktionsgleichung
[Mg].Cl[CH:3]1[CH2:12][N:11]2[CH:6]([CH2:7][CH2:8][CH2:9][CH2:10]2)[CH2:5][CH2:4]1.[Cl:13][C:14]1[CH:27]=[CH:26][C:25]2[S:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17](=[O:28])[C:16]=2[CH:15]=1.[Cl-].[NH4+]>C(Br)C.O1CCCC1>[Cl:13][C:14]1[CH:27]=[CH:26][C:25]2[S:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]([CH:3]3[CH2:12][N:11]4[CH:6]([CH2:7][CH2:8][CH2:9][CH2:10]4)[CH2:5][CH2:4]3)([OH:28])[C:16]=2[CH:15]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
Several drops of ethyl bromide were added to a stirred suspension of 1.29 g. (0.054 g.-atom) of magnesium turnings in 5 ml. of tetrahydrofuran under a nitrogen atmosphere. After the reaction began 9.3 g. (0.054 mole) of 3-chloroquinolizidine in 100 ml. of tetrahydrofuran was added. After the addition was completed the mixture was stirred and refluxed for one hour and cooled to 0° C. To the chilled suspension of the Grignard reagent was added a solution of 12.55 g. (0.051 mole) of 2-chloro-9-thioxanthone in 300 ml. of tetrahydrofuran. The solution was stirred at 24° C. for two hours, poured into aqueous ammonium chloride and extracted with ether. The extracts were washed with water, dried and evaporated to give 2-chloro-9-(3-quinolizidinyl)-9-hydroxythioxanthene.
Aufarbeitung
- additionAfter the addition
- temperaturerefluxed for one hour
- additionwas added a solution of 12.55 g
- stirringThe solution was stirred at 24° C. for two hours
- extractionextracted with ether
- washThe extracts were washed with water
- customdried
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-7e97f4f7917a405781fe469772573c1d
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04089961
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