Propylamine → HCID 32911, compound
Reaction equation
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].C(=O)([O-])O.[K+].[CH2:15]([NH2:18])[CH2:16][CH3:17]>CC(C)=O.O>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([NH:18][CH2:15][CH2:16][CH3:17])[N:7]=1Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 0 °C
Procedure
Cyanuric chloride (1) (36.9 g, 0.2 mole) was dissolved in acetone (600 ml) and cooled in an ice/acetone bath. Potassium hydrogen carbonate (25.03 g, 0.25 mole) was dissolved in water (150 ml) with propylamine (11.82 g, 0.2 mole) and added dropwise to the solution of (1) while maintaining the temperature below 0° C. The mixture was stirred for 1 hour at 0° C. and then stirred for 1 hour at room temperature. The acetone was evaporated off under reduced pressure and the residue (300 ml) was poured into water (11). The resulting white solid was filtered, washed with water and dried under vacuum.
Workup
- temperaturecooled in an ice/acetone bath
- temperaturewhile maintaining the temperature below 0° C
- stirringstirred for 1 hour at room temperature
- customThe acetone was evaporated off under reduced pressure
- additionthe residue (300 ml) was poured into water (11)
- filtrationThe resulting white solid was filtered
- washwashed with water
- customdried under vacuum
Sources & evidence
- ORD record
- ord-fb60067b72924a4bbe4e9abf7372dc8c
- Source dataset
- uspto-grants-1999_02
- Patent number
- US05869222
Reaction notes
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