Reaction equation
O[CH2:2][CH2:3][C:4]([NH2:6])=[O:5].[CH:7]1(N)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.N>>[CH:7]1([NH:6][C:4](=[O:5])[CH:3]=[CH2:2])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1Participants
4
Conditions
- Temperature
- 164 °C
Procedure
59 g of β-hydroxypropionamide and 69.4 g of cyclohexylamine were heated with 50 mg of 2,6-di-t-butyl-pcresol for 5 hours in a temperature range of 130°-170° C. until the evolution of ammonia was complete. After adding 2.5 g of polyphosphoric acid the reaction mixture was maintained at 164° C. for 1 hour and then distilled in a water jet vacuum. The main run was taken off between 140° and 160° C. at 11 bar and crystallized in the receiver.
Workup
- distillationdistilled in a water jet vacuum
- customwas taken off between 140° and 160° C. at 11 bar
- customcrystallized in the receiver
Sources & evidence
- ORD record
- ord-2affe934e98d48669833c62c048622d8
- Source dataset
- uspto-grants-1980_12
- Patent number
- US04237067
Linked notes
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