Chlorosuccinimide → 935777-25-6
Reaction equation
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[N:7][C:6]([NH2:9])=[CH:5][CH:4]=1.[Cl:12]N1C(=O)CCC1=O>C(#N)C>[Cl:12][C:5]1[CH:4]=[C:3]([C:2]([F:1])([F:10])[F:11])[N:8]=[N:7][C:6]=1[NH2:9]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 70 °C
Procedure
A mixture of D6 (4.0 g, 24.5 mmol) and N-chlorosuccinimide (3.3 g, 24.5 mmol) in acetonitrile (160 ml) was heated at 70° C. for 18 h. After this period, the reaction was cooled to room temperature and the solvents evaporated in vacuo. The crude residue was purified by column chromatography (silica; 3%-5% methanol/dichloromethane) to give D7 (1.6 g, 33%). C5H3ClF3N3 requires 197; Found 198 (MH+)
Workup
- waitAfter this period
- temperaturethe reaction was cooled to room temperature
- customthe solvents evaporated in vacuo
- customThe crude residue was purified by column chromatography (silica; 3%-5% methanol/dichloromethane)
Sources & evidence
- ORD record
- ord-90b970214969402fb06786c7750dffe9
- Source dataset
- uspto-grants-2015_01
- Patent number
- US08940743B2
Reaction notes
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