Dimethylformamide → HCID 86744038, compound
Reaction equation
Br[C:2]1[CH:3]=[C:4]([C:16]([CH3:20])([CH3:19])[C:17]#[N:18])[C:5]([CH2:13]C#N)=[C:6]([C:8]([CH3:12])([CH3:11])[C:9]#[N:10])[CH:7]=1.[NH:21]1[CH:25]=[N:24][CH:23]=[N:22]1.[CH3:26][N:27](C)C=O>O>[C:26]([C:2]1[CH:3]=[C:4]([C:16]([CH3:20])([CH3:19])[C:17]#[N:18])[C:5]([CH2:13][N:21]2[CH:25]=[N:24][CH:23]=[N:22]2)=[C:6]([C:8]([CH3:11])([CH3:12])[C:9]#[N:10])[CH:7]=1)#[N:27]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 2,2'-[5-bromocyanomethyl-1,3-phenylene]di(2-methylpropiononitrile) (0.33 g), 1,2,4-triazole (0.34 g) and dimethylformamide (2 ml) was stirred at 50° for 24 h. The mixture was treated with water (20 ml), and extracted with ethyl acetate, and the extract was dried and evaporated to dryness under reduced pressure. The residue was purified by flash chromatography, using methanol (3% by volume) in dichloromethane as eluant, to give 2,2'-[5-cyano(1H-1,2,4-triazol-1-yl)methyl-1,3-phenylene]di(2-methylpropiono-nitrile), characterised as the hydrochloride salt, mp 148°-151°.
Workup
- extractionextracted with ethyl acetate
- customthe extract was dried
- customevaporated to dryness under reduced pressure
- customThe residue was purified by flash chromatography
Sources & evidence
- ORD record
- ord-be510770424748eab902e0c29e448c7e
- Source dataset
- uspto-grants-1990_06
- Patent number
- US04935437
Reaction notes
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