Phenyl isocyanate → HCID 178493809, compound
Reaction equation
[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[O:8]C.N1CCOCC1.C1(N=C=O)C=CC=CC=1>C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[OH:8]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr, and cooled to 0° C. To the reaction mixture was added phenyl isocyanate (73.8 mL) at 0° C., and the mixture was stirred at the same temperature for 30 min, and diluted with ethyl acetate. The resulting solid was removed by filtration. The filtrate was concentrated, and the residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate) to give the title compound (9.61 g).
Workup
- customThe resulting solid was removed by filtration
- concentrationThe filtrate was concentrated
- customthe residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate)
Sources & evidence
- ORD record
- ord-431a0c70d78e4904b73982c60d4ce753
- Source dataset
- uspto-grants-2015_07
- Patent number
- US09090586B2
Reaction notes
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