Reaktionsgleichung
Br[CH2:2][C:3]([C:5]1[CH:14]=[CH:13][C:12]2[C:11]([CH3:16])([CH3:15])[CH2:10][CH2:9][C:8]([CH3:18])([CH3:17])[C:7]=2[CH:6]=1)=O.C(OC([N:26]1[CH2:31][CH2:30][CH:29]([C:32](=[S:34])[NH2:33])[CH2:28][CH2:27]1)=O)(C)(C)C>C(O)C>[CH3:15][C:11]1([CH3:16])[CH2:10][CH2:9][C:8]([CH3:18])([CH3:17])[C:7]2[CH:6]=[C:5]([C:3]3[N:33]=[C:32]([CH:29]4[CH2:30][CH2:31][NH:26][CH2:27][CH2:28]4)[S:34][CH:2]=3)[CH:14]=[CH:13][C:12]1=2Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
6.12 g (12.28 mmol) of 2-bromo-1-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethanone and 3 g (12.28 mmol) of 4-thiocarbamoylpiperidine-1-carboxylic acid tert-butyl ester were suspended in 50 ml of ethanol and refluxed overnight. The reaction mixture was cooled and evaporated. The residue was slurried using a little EA and PE, digested and filtered off with suction. The solid was suspended in 180 ml of EA, washed with 60 ml of a saturated sodium hydrogencarbonate solution. The organic phase was dried over sodium sulfate, filtered and evaporated.
Aufarbeitung
- temperaturerefluxed overnight
- temperatureThe reaction mixture was cooled
- customevaporated
- filtrationfiltered off with suction
- washwashed with 60 ml of a saturated sodium hydrogencarbonate solution
- dry with materialThe organic phase was dried over sodium sulfate
- filtrationfiltered
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-91233daecc434ed0a6e7033d6d8cfde8
- Quelldatensatz
- uspto-grants-2014_12
- Patentnummer
- US08907098B2
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