Triethylamine → HCID 21487069, compound
Reaction equation
C([N:3]([CH2:6][CH3:7])CC)C.Cl[C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][N:10]=1>C(O)C>[CH2:6]([NH:3][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][N:10]=1)[CH2:7][CH2:11][CH2:12][CH2:13][CH3:14]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
101 g of triethylamine and subsequently 50 g of n-hexylamino are placed into 600 ml of distilled anhydrous ethanol. An amount of 79 g of 2-chloro-5-nitropyridine is added portionwise at room temperature in the course of 15 minutes. The mixture is then heated to reflux temperature, whereby it goes into solution at 60° C. The solution is stirred for 24 hours at the reflux temperature and afterwards cooled to room temperature; the solution is poured into ice/water, and the formed precipitate filtered off. The 2-n-hexylamino-5-nitropyridine obtained after recrystallisation from ethanol/water melts at 56°-57° C.
Workup
- temperatureThe mixture is then heated
- temperatureto reflux temperature, whereby it
- customgoes into solution at 60° C
- filtrationthe formed precipitate filtered off
Sources & evidence
- ORD record
- ord-8cc533027ad54b549f27f9a441dae452
- Source dataset
- uspto-grants-1977_01
- Patent number
- US04001254
Reaction notes
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