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CAS No. : | 1455091-10-7 | MDL No. : | MFCD29075436 |
Formula : | C17H13NO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | YTWDBRIDKWWANA-UHFFFAOYSA-N |
M.W : | 295.29 | Pubchem ID : | 86709142 |
Synonyms : |
|
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 |
---|---|---|
300 mg | In ethanol; for 18h;Reflux; | To a solution of the 3-amino-2,2-dimethyl-propionic acid ethyl ester (598 mg, 4.12 mmol) in EtOH (9.1 mL) at r.t. were added 4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (81 1 mg, 2.75 mmol) to give suspension solution, the reaction mixture was allowed to reflux for 18 h. After cooled to rt, the solvent was evaporated in vacuo, the crude was purified by silica gel chromatography to give 300 mg of title compound as a yellow oil: MS (m/z) 409.0 (M+l)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78.8% | With sodium methylate; In methanol; dimethyl sulfoxide; at 20℃; for 2h; | Ice bath,Sodium methoxide (12.70 g 2.34.60 mmol)Of methanol (40 mL)The solution was added dropwise to a solution of methyl 2 - (((N- (2-methoxy-2-oxoethyl) -4-methylphenyl) sulfonyl) methyl) -4-phenoxybenzoate 18.90 g, 39.10 mmol)In dimethyl sulfoxide (82 mL), after completion of the dropwise addition,The reaction solution was stirred at room temperature for 2 hours.The methanol was removed under reduced pressure,Add water (50 mL) dilute the concentrate,The pH was adjusted to pH = 10 with 1N dilute hydrochloric acid.Ethyl acetate (100 mL x 3)The organic layer was washed with water (100 mL) and saturated brine (100 mL), respectively,Dried over anhydrous sodium sulfate. Concentrated under reduced pressure,The concentrate was subjected to column separation to give 9.1 g of a white solid in a yield of 78.8%. |
72.9% | With sodium methylate; In methanol; dimethyl sulfoxide; at 20℃; for 0.5h; | To a mixture of 2- [Methoxycarbonylmethyl-(toluene-4-sulfonyl)-amino]-methyl}-4- phenoxy-benzoic acid methyl ester (14.0 g, 28.1 mmol) in DMSO (56 mL) was slowly added 30% NaOMe in MeOH (15.3 mL, 84.3 mmol). The resultant mixture was stirred at room temperature for 30 min and poured into 200 mL of ice and water. It was slowly acidified by cone. HCl aq. solution (10 mL) and then extracted with EtOAc. Organic layer was washed with 3% NaHC03 solution, water and brine, and was dried over Na2SO/t, filtered and concentrated. Crude produce was purified by silica gel chromatography to provide the title compound 6.05 g (20.5 mmol) in 72.9% yield. lH NMR in CDCI3, delta in ppm: 1 1.7 (s, 1 H), 8.59 (s, 1 H), 8.36 (d, 1 H, J = 9.2 Hz), 7.55-7.1 (m, 7 H), 4.07 (s, 3 H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90.7% | With N-Bromosuccinimide; In dichloromethane; for 2h; | Add dichloromethane (2L) and <strong>[1455091-10-7]4-hydroxy-7-phenoxyisoquinoline-3-carboxylic acid methyl ester</strong> (200.00g, 0.68mol) to the reaction flask in sequence, after stirring,Add N-bromosuccinimide (NBS) (126.60g, 0.71mol) into the reaction bottle, and after the end of the addition, react for 2 hours.After distilling off about half of the methylene chloride under reduced pressure, methanol (2L) was added, and the crystal was stirred for 1h.After filtration, the filter cake was blow-dried to obtain 1-bromo-<strong>[1455091-10-7]4-hydroxy-7-phenoxyisoquinoline-3-carboxylic acid methyl ester</strong> (229.67g, yield 90.7%, purity 98.98%). |
86.4% | With 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione; In methanol; at 5℃;Reflux; | Methyl 4-hydroxy-7-phenoxyisoquinoline-3-carboxylate (Compound A) 2.95 g,The stirring temperature of the ice water bath was lowered to 5-10 C, and 1.57 g of 1,3-dibromo-5,5-dimethylhydantoin was added, and methanol was used as a solvent, and the reaction was refluxed for 4-6 h.The TLC monitors the reaction to the starting material completely, 0~10 C, suction filtration, the filter cake is rinsed with methanol, and dried under vacuum.A pale yellow solid, Compound B (yield 86.4%, purity 98.5%) was obtained. |
58% | With N-Bromosuccinimide; dibenzoyl peroxide; In tetrachloromethane; for 1h;Reflux; | A mixture of 4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (6.0 g, 20.32 mmol), N-bromosuccinimide (3.80 g, 21.33 mmol) and benzoyl peroxide (246 mg, 1.01 mmol) in CCI4 was refluxed for 1 h. Solid was filtered off through a plug of silica gel. Filtrate was concentrated and purified by silica chromatography, eluting with EtOAc. All fractions contain the desired product was combined and concentrated. Residue was suspended in 150 mL of (3/1) MeOH/EtOAc and was refluxed for 1 h. After cooled, solid was collected, rinsed with MeOH and dried on vacuo to provide the title compound 4.42 g (1 1.8 mmol) in 58% yield as a white solid. H NMR in CDC13, delta ppm: 1 1.7 (s, 1 H), 8.36 (d, 1 H, J = 9.2 Hz), 7.63 (d, 1 H, J = 2.4 Hz), 7.55-7.10 (m, 6 H), 4.06 (s, 3 H). |
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