HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 60112889, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1,3-Propanediamine, N1,N1,N3-trimethyl- | HCID 78302 | — |
| Reactant | HCID 60112821 | HCID 60112821 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60112889 | HCID 60112889 | — |
Reaction Steps
To an excess of phosgene dissolved in toluene are added at 0° C. 41.5 μl (0.283 mmol) N,N,N′-trimethyl-1,3-propanediamine. After 5 minutes the solvent is evaporated and the residue is dissolved in 2 ml dichloromethane. Triethylamine (79.2 μl, 0.566 mmol) and a solution of 100 mg (0.236 mmol) 1-(4-hydroxy-benzyl)-4-(4-isopropyl-phenyl)-6-prop-2-ynyloxy-1H-quinazolin-2-one in 2 ml dichloromethane are added at 0° C. After stirring for 20 h at rt aqueous ammonia and 0.1 M NaOH are added. The title compound is obtained by extraction with dichloromethane followed by reversed phase preparative HPLC.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476286B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-fc17dec741ca4507bcccc0aca0fe05a0 |
| Source note | uspto-grants-2013_07 |