Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 21183891 | HCID 21183891 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21183965 | HCID 21183965 | 85.4% |
Reaction Steps
75 ml of thionyl chloride and 150 ml of acetonitrile were added to 3.8 g (0.0086 mol) of 2-(4-carbamoylpiperidino)-4-(3, 4-methylenedioxybenzyl)amino-6-chloroquinazoline. The mixture thus obtained was heated under reflux for one hour. The reaction mixture was distilled under a reduced pressure to remove the solvent. A saturated aqueous solution of sodium hydrogencarbonate and triethylamine were added to the residue and the resultant mixture was etracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, filtered and distilled under a reduced pressure to remove the solvent. The obtained residue was purified by a silica gel column chromatography (ethyl acetate-n-hexane) and recrystallized from chloroform-n-hexane to give 3.1 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05801180 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-708a51980f3a4feb873583547ab52fb4 |
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| Source note | uspto-grants-1998_09 |
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