Bromine → HCID 20154322, compound
Reaction equation
[C:1]([NH:4][CH2:5][C:6]1[S:7][C:8]([C:11](=[O:13])[CH3:12])=[CH:9][CH:10]=1)(=[O:3])[CH3:2].[Br:14]Br>C(Cl)(Cl)Cl>[C:1]([NH:4][CH2:5][C:6]1[S:7][C:8]([C:11](=[O:13])[CH2:12][Br:14])=[CH:9][CH:10]=1)(=[O:3])[CH3:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 40.3 g of 2-acetylaminomethyl-5-acetylthiophene in 500 ml of chloroform is added dropwise bromine under cooling with ice at 5°-10° C., and the mixture is stirred at room temperature for 30 minutes. After the resulting mixture is washed with water, dried over anhydrous magnesium sulfate and concentrated, the residue is recrystallized from ethanol to give 2-acetylaminomethyl-5-bromoacetylthiophene, melting at 129°-131° C.
Workup
- temperatureunder cooling with ice at 5°-10° C.
- washAfter the resulting mixture is washed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customthe residue is recrystallized from ethanol
Sources & evidence
- ORD record
- ord-28bb7dea11d641d7ba4c3d1b666db1b2
- Source dataset
- uspto-grants-1988_01
- Patent number
- US04720493
Reaction notes
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