HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Tetrachloride → HCID 18924988, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Benzenamine, 3-ethynyl- | HCID 104682 | — |
| Reactant | HCID 136008347 | HCID 136008347 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 18924988 | HCID 18924988 | — |
Reaction Steps
6-Chloro-7-(2-methoxyethylsulfanyl)-quinazolin-4-one (200 mg, 0.739 mmol), triphenylphosphine (427 mg, 1.63 mmol) and 0.7 mL of carbon tetrachloride were refluxed in 4 ml of 1,2-dichloroethane for 4 hours, concentrated in vacuo to a residue, diluted with 4 mL of isopropyl alcohol and 3-ethynylaniline (129 mg, 1.104 mmol) and refluxed for 16 hours. The hot reaction mixture was filtered to isolate crude product which was column chromatographed on silica gel eluted with 5% methanol in chloroform. Fractions containing the pure product were concentrated in vacuo to afford the title product as a solid; 23 mg (8.4%); mp 230°-232° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE041065E1 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-4cb3f681bbb8432888b95e4f9aabd7b4 |
| Source note | uspto-grants-2009_12 |