HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 11776699, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 10406630 | HCID 10406630 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11776699 | HCID 11776699 | 80% |
Reaction Steps
A solution of 1.4 g (4.11 mmol) of 6-chloro-4-cyclopropyl-4-ethynyl-3,4-dihydro-1-(p-methoxybenzyl)quinazolin-2(1H)-one in 5 mL of CH2Cl2 was treated with 10 mL of trifluoroacetic acid (Aldrich) under N2 overnight at r.t. The reaction was concentrated by rotovap under reduced pressure and the residue partitioned between ethyl acetate and 10% citric acid. The organic layer was washed with water, brine, dried over MgSO4 and the solvents removed to give an oil which was flash chromatographed on SiO2 using 95:5 CHCl3 --CH3OH to give a foam. Trituration of this material with ether gave 720 mg (80%) of the title compound as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05457201 |
| Source dataset | uspto-grants-1995_10 |
| ORD ID | ord-219f890163c44f66b38a93da8d36d092 |
| Source note | uspto-grants-1995_10 |