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CAS No. : | 1029689-82-4 | MDL No. : | MFCD08460905 |
Formula : | C11H14ClNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | COQHHVHUWVSLQP-UHFFFAOYSA-N |
M.W : | 227.69 | Pubchem ID : | 45074000 |
Synonyms : |
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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 |
---|---|---|
With potassium carbonate;sodium iodide; In N,N-dimethyl acetamide; at 160.0℃; for 12.0h; | Example 11; <n="71"/>Synthesis of methyl 2-f6.7.8-trimethoxyquinazoline-4-vD- 1.2.3.4- tetrahycroisoquinoline-8-carboxylate; [00214] Methyl 1, 2,3 ,4-tetrahydroisoquinoline-8-carboxy late hydrochloride (268 mg,1.18 mmol), N,N-dimethylacetamide (14.6 mL, 0.158 mol), 4-chloro-6,7,8- trimethoxyquinazoline (300 mg, 1.18 mol), sodium iodide (80 mg, 0.0005 mol), and potassium carbonate (407 mg, 02.94 mol) were combined and heated at 160 0C for 12 hr. The crude product was purified by preparative HPLC with a C 18 column using acetonitrile: water (with 0.1% formic acid) as eluant with a gradient from 10:90 (v/v) to 80:20 (v/v) at a flow rate of 45 mL/min to give methyl 2-(6,7,8-trimethoxyquinazoline-4-yl)- l,2,3,4-tetrahycroisoquinoline-8-carboxylate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With caesium carbonate; In N,N-dimethyl acetamide; at 120℃;Inert atmosphere; | Example 67A 2-(5-bromo-6-(tert-butoxycarbonyl)pyridin-2-yl)-1,2,3,4-tetrahydroisoquinoline-8-carboxylic acid A solution of methyl 1,2,3,4-tetrahydroisoquinoline-8-carboxylate, hydrochloric acid (13.6 g), <strong>[1235036-15-3]tert-butyl 3-bromo-6-chloropicolinate</strong> (17.4 g) and cesium carbonate (39 g) were stirred together in N,N-dimethylacetamide (110 mL) and heated at 120 C. under nitrogen overnight. The reaction mixture was cooled, diluted with water and extracted with ethyl acetate. The organic layer was washed with brine and the combined aqueous layers were back-extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated. Silica gel chromatography using 20-100% ethyl acetate in hexanes provided the title compound. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of methyl l,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride (12.37 g) and Example 1.1.11 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL). The mixture was stirred at 50C for 24 hours. The mixture was then diluted with ethyl acetate (500 mL), washed with water and brine, and dried over NaaSOzi. Filtration and evaporation of the solvent gave a residue that was purified by silica gel chromatography, eluting with 20% ethyl acetate in heptane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. | |
With N-ethyl-N,N-diisopropylamine; In hexane; dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of <strong>[1029689-82-4]methyl 1,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride</strong> (12.37 g) and Example 1.4.4 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL). The mixture was stirred at 50 C. for 24 hours. The mixture was diluted with ethyl acetate (500 mL), washed with water and brine, and dried over Na2SO4. After filtration and evaporation of the solvent, the crude material was purified via silica gel column chromatography, eluting with 20% ethyl acetate in hexane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. | |
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | [000516] To a solution of methyl l,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride (12.37 g) and Example 1.1.10 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL), and the mixture was stirred at 50 C for 24 hours. The mixture was then diluted with ethyl acetate (500 mL) and washed with water and brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with 20% ethyl acetate in hexane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. |
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of methyl l,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride (12.37 g) and Example 1.4.4 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine(12 mL). The mixture was stirred at 50 C for 24 hours. The mixture was diluted with ethyl acetate (500 mL), washed with water and brine, and dried over Na2S04. After filtration and evaporation of the solvent, the crude material was purified via silica gel column chromatography, eluting with 20% ethyl acetate in hexane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. | |
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of <strong>[1029689-82-4]methyl 1,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride</strong> (12.37 g) and Example 1.1.10 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL), and the mixture was stirred at 50 oC for 24 hours. The mixture was then diluted with ethyl acetate (500 mL) and washed with water and brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with 20% ethyl acetate in hexane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. | |
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of <strong>[1029689-82-4]methyl 1,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride</strong> (12.37 g) and Example 1.1.10 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL), and the mixture was stirred at 50 C. for 24 hours. The mixture was then diluted with ethyl acetate (500 mL) and washed with water and brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with 20% ethyl acetate in hexane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. | |
With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 50.0℃; for 24.0h; | To a solution of <strong>[1029689-82-4]methyl 1,2,3,4-tetrahydroisoquinoline-8-carboxylate hydrochloride</strong> (12.37 g) and Example 1.1.11 (15 g) in dimethyl sulfoxide (100 mL) was added N,N-diisopropylethylamine (12 mL). The mixture was stirred at 50 C. for 24 hours. The mixture was then diluted with ethyl acetate (500 mL), washed with water and brine, and dried over Na2SO4. Filtration and evaporation of the solvent gave a residue that was purified by silica gel chromatography, eluting with 20% ethyl acetate in heptane, to give the title compound. MS (ESI) m/e 448.4 (M+H)+. |
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