HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-oxo-N-[(3-piperazin-1-ylphenyl)methyl]-3,4-dihydroquinazoline-2-carboxamide dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | 1,1-Dimethylethyl 4-[3-({[(4-oxo-3,4-dihydroquinazolin-2-yl)carbonyl]amino}methyl)phenyl]piperazine-1-carboxylate | HCID 136054488 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 4-oxo-N-[(3-piperazin-1-ylphenyl)methyl]-3,4-dihydroquinazoline-2-carboxamide dihydrochloride | HCID 136380965 | 97% |
Reaction Steps
To a suspension of 1,1-dimethylethyl 4-[3-({[(4-oxo-3,4-dihydroquinazolin-2-yl)carbonyl]amino}methyl)phenyl]piperazine-1-carboxylate obtained in Reference Example 115 (2.40 g, 6.86 mmol) in ethyl acetate (10 mL)-THF (50 ml)-methanol (40 mL) was added 4N hydrogen chloride-ethyl acetate (10.4 mL), and the mixture was stirred at room temperature for 4 hr, and then at 50° C. for 2 hr. Diethyl ether (about 100 mL) was added to the reaction mixture, and the precipitated solid was collected by filtration to give the title compound as a white powder (2.18 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915267B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-07c21c902cc3492c8a16e4decdddde7c |
| Source note | uspto-grants-2011_03 |