Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 13544732 | HCID 13544732 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53446128 | HCID 53446128 | — |
Reaction Steps
25 gms, 0.77 moles of N-(4-amino-6,7-dimethoxyquinazol-2-yl)-N-methyl-2-cyanoethylamine hydrochloride, 25 gms of Raney-Nickel and 500 ml of 9.8% methanolic ammonia solution were charged in an autoclave. The reaction mixture was hydrogenated at 70° C. under a pressure of 5 kg/cm2 (70 psi) for 2 hours. The reaction mass was cooled to room temperature, filtered on hyflo bed and washed with 200 ml methanol. The solvent was distilled under reduced pressure. The residue obtained was stirred in 50 ml methylene chloride and concentrated under reduced pressure at 40° C. The residue was dissolved in 200 ml isopropanol and acidified to pH 1-2 with isopropanolic HCl. The N-(4-amino-6,7-dimethoxyquinazol-2-yl)-N-methyl propylenediamine hydrochloride obtained was isolated by filtration and dried under suction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08716476B2 |
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| Source dataset | uspto-grants-2014_05 |
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| ORD ID | ord-bf82aa805ff84b35ac0ec55f92a4cbff |
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| Source note | uspto-grants-2014_05 |
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