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CAS No. : | 202475-60-3 | MDL No. : | MFCD01862614 |
Formula : | C16H15N3O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HOZUXBLMYUPGPZ-UHFFFAOYSA-N |
M.W : | 297.31 | Pubchem ID : | 3794 |
Synonyms : |
Jak3 inhibitor I;WHI-P131;WHI-P131, WHI P-131, WHI P131, Janex 1
|
Chemical Name : | 4-((6,7-Dimethoxyquinazolin-4-yl)amino)phenol |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | In isopropyl alcohol; at 85℃; for 2h; | A mixture of <strong>[13790-39-1]4-chloro-6,7-dimethoxyquinazoline</strong> (1.00 g, 4.452 mmol, 1.00 equiv) and 4-aminophenol (583 mg, 5.342 mmol, 1.20 equiv) in isopropanol (15 mL) was stirred at 85C for 2 h. After cooled to room temperature, the solid was collected by filtration, washed with methanol (15 mL x 2) and dried in vacuo to give 1.30 g (98%) of 4-(6,7-dimethoxyquinazolin-4- ylamino)phenol as an off-white solid. 1H-NMR (300 MHz, DMSO-rL, ppm): d 11.07 (s, 1H), 9.66 (s, 1H), 8.70 (s, 1H), 8.22 (s, 1H), 7.45-7.40 (m, 2H), 7.32 (s, 1H), 6.88-6.82 (m, 2H), 3.99 (s, 3H), 3.97 (s, 3H). |
With triethylamine; In ethanol; | 4-(4'-hydroxyphenyl)amino-6,7-dimethoxyquinazoline was prepared by the condensation of <strong>[13790-39-1]4-chloro-6,7-dimethoxyquinazoline</strong> with 4-aminophenol as outlined below in Scheme 2 above. Specifically, a mixture of <strong>[13790-39-1]4-chloro-6,7-dimethoxyquinazoline</strong> (448 mg, 2 mmols) and 4-aminophenol (2.5 mmols) in EtOH (20 ml) was heated to reflux. After refluxing for 4 to 24 hours, an excess amount of Et3N was added, and the solvent was concentrated to give the crude product which was recrystallized from DMF. | |
Heating; | General procedure: 4-Chloro-6,7-dimethoxyquinazoline 3 and the required nucleophile were heated in solvent either thermally or using microwave heating until no further reaction was observed. On cooling, the hydrochloride salt was isolated by filtration. Alternative isolation procedures were employed if precipitation did not occur. Additional purification by preparative HPLC or flash column chromatography was employed in some cases. Spectroscopic data for compounds 4 [13], 6-9 [14-16], 20-21 [13], 25 [13], 28 [17] and 30 [18] are in agreement with those reported in the literature. |