Isopropanol → HCID 178479150, compound
Reaction equation
[OH:1][CH:2]([CH2:5][NH2:6])[CH2:3][NH2:4].[ClH:7].[NH2:8][C:9](N)=N.CC(O)C>CC#N>[ClH:7].[NH:8]=[C:9]1[NH:6][CH2:5][CH:2]([OH:1])[CH2:3][NH:4]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 140 °C
Procedure
A mixture of 2-hydroxy -1,3-diaminopropane (9.80 g, 108 mmol) and guanidine hydrochloride (10.4 g, 108 mmol) in a 100 mL RBF was heated at 140° C. under nitrogen for 5 h. The reaction mixture, while under vigorous stirring, was let cooled to 100° C. whereby a mixture of iPrOH (5 mL) and CH3CN (5 mL) were added, resulting in the formation of a slurry. After cooled to room temperature, the mixture was filtered and the solid was washed with additional CH3CN (total 30 mL). The solid was further dried under vacuum to yield a white solid. 1H NMR (400 MHz, D2O): 4.21 (m, 1 H), 3.34 (dt, J 15.2, 2.8, 2H), 3.22 (dt, J 15.2, 2.8).
Workup
- temperatureThe reaction mixture, while under vigorous stirring, was let cooled to 100° C. whereby
- additionwere added
- customresulting in the formation of a slurry
- temperatureAfter cooled to room temperature
- filtrationthe mixture was filtered
- washthe solid was washed with additional CH3CN (total 30 mL)
- customThe solid was further dried under vacuum
- customto yield a white solid
Sources & evidence
- ORD record
- ord-a93d0ed17ef24fb492871f8e95ea8aed
- Source dataset
- uspto-grants-2009_03
- Patent number
- US07504403B2
Reaction notes
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