Ethyl isocyanate → 1-(3-Chloropyrido[2,3-b]pyrazin-6-yl)-3-ethylurea
Reaction equation
[Cl:1][C:2]1[N:7]=[C:6]2[N:8]=[C:9]([NH2:12])[CH:10]=[CH:11][C:5]2=[N:4][CH:3]=1.[CH2:13]([N:15]=[C:16]=[O:17])[CH3:14]>N1C=CC=CC=1>[Cl:1][C:2]1[N:7]=[C:6]2[N:8]=[C:9]([NH:12][C:16]([NH:15][CH2:13][CH3:14])=[O:17])[CH:10]=[CH:11][C:5]2=[N:4][CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 75 °C
Procedure
100 mg 3-chloropyrido[2,3-b]pyrazine-6-yl-amine (0.55 mmol) was presented in 5 ml predried pyridine and add 44 μL ethyl isocyanate (0.55 mmol) at room temperature. The mixture was stirred at 75° C. and then a total of 132 μL ethyl isocyanate (1.65 mmol) was added again over 18 hours to the reaction mixture in small amounts. Then the volatile components were removed in vacuum. The resulting solid was cleaned through column chromatography on silica gel (solvent dichloromethane/methanol). A light yellow solid was obtained.
Workup
- customThen the volatile components were removed in vacuum
- customA light yellow solid was obtained
Sources & evidence
- ORD record
- ord-fc0e31b0b0e94992849f900663b35993
- Source dataset
- uspto-grants-2015_01
- Patent number
- US08937068B2
Reaction notes
Loading…