Reaction equation
[C:1]([CH2:3][NH:4][C:5](=[O:21])[C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([NH:13][C:14]([CH3:16])=[O:15])=[CH:8][C:7]=1[O:17]C(=O)C)#[N:2].[CH2:22]([NH:24][CH2:25][CH2:26]N)[CH3:23]>C(=S)=S>[CH2:22]([N:24]1[CH2:25][CH2:26][N:2]=[C:1]1[CH2:3][NH:4][C:5](=[O:21])[C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([NH:13][C:14]([CH3:16])=[O:15])=[CH:8][C:7]=1[OH:17])[CH3:23]Participants
4
Procedure
143 g of N-(cyanomethyl) 2-acetoxy 4-acetamino 5-chlorobenzamide was introduced into a one liter balloon flask provided with sealed agitator, a reflux condenser on which there was disposed a bubble counter containing vaseline oil, a thermometer and a dropping funnel. Thereafter, 123 g of N-ethyl ethylene diamine were rapidly added dropwise. The reaction was exothermic. The temperature rose to 110° C. and the amount of gas evolved was substantial. A thick solution was obtained. The solution was heated to temperature of 120° and then, after 25 minutes of heating, drops of carbon disulphide were added and the temperature was then maintained at 120° for a further period of 20 minutes until the gas ceased to be evolved.
Workup
- customprovided
- customwith sealed agitator, a reflux condenser on which there
- additioncontaining vaseline oil
- customrose to 110° C.
- customA thick solution was obtained
- temperatureThe solution was heated to temperature of 120°
- temperatureafter 25 minutes of heating
- temperaturethe temperature was then maintained at 120° for a further period of 20 minutes until the gas
Sources & evidence
- ORD record
- ord-d3af57d45db54dd4948e9b937a0ee8dc
- Source dataset
- uspto-grants-1987_10
- Patent number
- US04703055
Linked notes
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