Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Reactant | N4-(3-Bromophenyl)quinazoline-4,6-diamine | HCID 5328042 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 178527248 | HCID 178527248 | 54% |
Reaction Steps
To a stirred solution of 6-amino-4-[(3-bromophenyl)amino]quinazoline (J Med Chem, 1995;38:3482) (0.30 g, 0.95 mmol) in THF (20 mL) under nitrogen was added Et3N (3.5 mol eq., 3.33 mmol, 245 μL), a catalytic amount of DMAP and chloroethanesulfonyl chloride (1.2 mol eq., 1.14 mmol, 119 μL) dropwise. The reaction was stirred at 25° C. for 1 hour and then diluted with saturated NaHCO3 and extracted with EtOAc. The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, concentrated under reduced pressure, and chromatographed on silica gel eluting with MeOH/CH2Cl2/EtOAc (3:47:50). Crystallization from CH2Cl2/hexane gave N-[4-[(3-bromophenyl)amino]-quinazolin-6-yl]vinylsulfonamide (210 mg, 54%) as a cream powder, mp 217° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06602863B1 |
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| Source dataset | uspto-grants-2003_08 |
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| ORD ID | ord-362b27af35714b9fa36c65ac4b92269a |
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| Source note | uspto-grants-2003_08 |
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