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发布于:2023-7-19 22:34:17  访问:45 次 回复:0 篇
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Ayer was washed with brine h2o, dried
Ayer was washed with brine drinking water, dried over sodium Rhod-2 AM supplier sulphate and evaporated on rotary evaporator to afford to pay for the ultimate compounds 5a-o.N-Desmethylclozapine custom synthesis synthesis of 2-chloro-1-(three,Cy2 Technical Information 4-dihydro-6,7-dimethoxyisoquinolin2(1H)-yl)ethanone (6)Chloroacetyl chloride two (two.24 g, twenty mmol) was additional dropwise to your ice cooled stirring answer of commencing substance 4 (four.6 g, twenty mmol) in DCM, in a round-bottom flask working with triethyl amine (seven.0 ml, fifty mmol,) as base (Plan 2). The microwave oven model Cata RI was programmed to three hundred W at one hundred for two to four.5 min. The reaction was monitored making use of TLC. Right after completion of reaction, ice h2o was added to the response combination which resulted the precipitation of your item. The sound solution was filtered off and washed with extra chilly water and dried to afford to pay for merchandise 8a. Comparable apporoach was followed for that synthesis of rest of the compounds (8b-o).The spectral characterization from the synthesized derivatives 2-(six,7-dimethoxy-3,4-dihydroisoquinolin-2(1H)-yl)-Nphenylacetamide (5a)Produce 78 ; white sound, MF: C20H24N2O3; MW: 340.eighteen; MP: 131?33 ; IR (KBr, , cm-1): PubMed ID:http://www.ncbi.nlm.nih.gov/pubmed/?term=7954456 3286, 3010, 2949, 2833, 1683, 1519, 1489, 1220, 1143, 1024; 1H NMR (four hundred MHz, CDCl3) 9.seventeen (s, 1H), seven.40 (d, J = eleven.8 Hz, 2H), seven.23 (t, J = 7.seven Hz, 1H), 6.95 (d, J = 7.six Hz, 1H), 6.sixty seven (s, 1H), 6.fifty five (s, 1H), three.88 (d, J = twelve.three Hz, 6H), 3.seventy four (d, J = seventeen.nine Hz, 2H), three.33 (s, 2H), 2.98 ?two.eighty (m, 4H), 2.36 (s, 3H); MS: m/z 341 (M + one).2-(six,7-dimethoxy-3,4-dihydroisoquinolin-2(1H)-yl)-N-ptolylacetamide (5d)Yield seventy three ; white reliable, MF: C19H22N2O3; MW: 326.16; MP: PubMed ID:http://www.ncbi.nlm.nih.gov/pubmed/10536014 151?54 ; IR (KBr, , cm-1): 3288, 3001, 2821, 2775, 1693, 1517, 1423, 1228, 1139, 1105; 1H NMR (400 MHz, CDCl3) 9.21 (s, 1H), 7.59 (dd, J = 8.six, 1.1 Hz, 2H), seven.39 ?7.31 (m, 2H), 7.14 (d, J = seven.4 Hz, 1H), six.sixty seven (s, 1H), six.55 (s, 1H), three.88 (d, J = twelve.2 Hz, 6H), three.seventy seven (s, 2H), 3.34 (s, 2H), 2.92 (s, 4H); MS: m/z 327 (M + 1).2-(six,7-dimethoxy-3,4-dihydroisoquinolin-2(1H)-yl)-N-otolylacetamide (5b)Generate 81 ; white stable, MF: C20H24N2O3; MW: 340.18; MP: 151?fifty three ; IR (KBr, , cm-1): 3267, 2943, 2827, 2779, 1685, 1517, 1462, 1253, 1196.Ayer was washed with brine drinking water, dried about sodium sulphate and
Ayer was washed with brine drinking water, dried in excess of sodium sulphate and evaporated on rotary evaporator to afford the ultimate compounds 5a-o.Synthesis of 2-chloro-1-(three,4-dihydro-6,7-dimethoxyisoquinolin2(1H)-yl)ethanone (six)Chloroacetyl chloride 2 (two.24 g, 20 mmol) was included dropwise towards the ice cooled stirring remedy of beginning content four (four.6 g, 20 mmol) in DCM, in the round-bottom flask working with triethyl amine (seven.0 ml, 50 mmol,) as base (Plan 2).
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