HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibenzylphosphate → Phosphoric acid dibenzyl ester 4-(4-tert-butyl-phenylamino)-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-2-ylmethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibenzylphosphate | HCID 4193600 | — |
| Reactant | [2-Chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine | HCID 58628208 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Phosphoric acid dibenzyl ester 4-(4-tert-butyl-phenylamino)-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-2-ylmethyl ester | HCID 9987362 | — |
Reaction Steps
Heat a solution of [2-chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine (417 mg, 0.89 mmol), Ag2O (308 mg, 1.33 mmol), and dibenzylphosphate (370 mg, 1.33 mmol) in acetonitrile at 70° C. for 18 hours. Dilute with additional acetonitrile and filter the hot solution through celite. Concentrate under reduced pressure to give a foam. Crystallize the crude product by dissolving in ether and slowly adding hexanes. Cool the resulting mixture on ice and collect the resulting solid via filtration to afford pure product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07432275B2 |
| Source dataset | uspto-grants-2008_10 |
| ORD ID | ord-593f3ae7d5fd4ab79e9f761f318487e0 |
| Source note | uspto-grants-2008_10 |