HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylamine → (3-{4-[3-Methyl-4-(6-methyl-pyridin-3-yloxy)-phenylamino]-quinazolin-6-yl}-prop-2-ynyl)-carbamic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylamine | HCID 7912 | — |
| Reactant | tert-butyl N-(prop-2-yn-1-yl)carbamate | HCID 11073648 | — |
| Reactant | 4-Quinazolinamine,6-iodo-n-[3-methyl-4-[(6-methyl-3-pyridinyl)oxy]phenyl]-,hydrochloride | HCID 66623307 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (3-{4-[3-Methyl-4-(6-methyl-pyridin-3-yloxy)-phenylamino]-quinazolin-6-yl}-prop-2-ynyl)-carbamic acid tert-butyl ester | HCID 66623656 | 98% |
Reaction Steps
A mixture of prop-2-ynyl-carbamic acid tert-butyl ester (2.65 g, 17.08 mmol) and (6-Iodo-quinazolin-4-yl)-[3-methyl-4-(6-methyl-pyridin-3-yloxy)-phenyl]-amine hydrochloride (8.2 g, 16.27 mmol), dichlorobis(triphenylphosphine) palladium (II) (570 mg, 0.81 mmol), copper iodide (154 mg, 0.81 mmol), and diisopropylamine (4.78 mL, 34.16 mmol) in anhydrous THF (80 mL) was stirred at room temperature for 5 hours. After concentration, the residue was dissolved in CH2Cl2 (100 mL), washed with aqueous NH4Cl and brine, dried over sodium sulfate, and concentrated to give the crude product (7.89 g, 98%) as a light yellow solid which was then used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07488823B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-7b0e188ab72444e0aa73e3afed79d0f7 |
| Source note | uspto-grants-2009_02 |