Tetrahydrothiophene → 1-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromide
Reaction equation
[S:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[Br:6][CH2:7][C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10]>C(#N)C>[Br-:6].[O:13]=[C:8]([C:9]([CH3:12])([CH3:11])[CH3:10])[CH2:7][S+:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Tetrahydrothiophene (11.8 g) was dissolved in 100 ml of acetonitrile, and 20 g of 1-bromo-3,3-dimethyl-2-butanone was slowly added to the above solution. The reaction solution was stirred at room temperature for two days, thereby a powder was precipitated. After adding 100 ml of ethyl acetate to the reaction solution, the powder was filtered out, washed with ethyl acetate and dried, thereby 24 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide was obtained.
Workup
- customa powder was precipitated
- additionAfter adding 100 ml of ethyl acetate to the reaction solution
- filtrationthe powder was filtered out
- washwashed with ethyl acetate
- customdried
Sources & evidence
- ORD record
- ord-11e4aee2f6d84e11a6513bca5d39247a
- Source dataset
- uspto-grants-2005_02
- Patent number
- US06858370B2
Reaction notes
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