N-(2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethyl)-3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide → N1,N3-bis(2-(2-(2-(2-(3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenylsulfonamido)ethoxy)ethoxy)ethoxy)ethyl)-2,2-dimethylmalonamide

関与物質

反応手順

Compound 182 was prepared from compound 28 and bis(2,5-dioxopyrrolidin-1-yl) 2,2-dimethylmalonate (prepared using the methods outlined in example 168) following the procedure outlined in example 175. The crude product (250 mg) was purified by Prep-HPLC with the following conditions: Column, C18 silica gel; mobile phase, MeCN/H2O/CF3COOH=39/100/0.05; Detector, UV 254 nm. This resulted in 152.3 mg (47%) of a TFA salt of N1,N3-bis(2-(2-(2-(2-(3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenylsulfonamido)ethoxy)ethoxy)ethoxy)ethyl)-2,2-dimethylmalonamide as a white solid. 1H-NMR (300 MHz, CDCl3, ppm): δ 7.92-7.89 (d, J=8.1 Hz, 2H), 7.79 (s, 2H), 7.69˜7.64 (m, 2H), 7.57-7.55 (d, J=7.5 Hz, 4H), 3.68 (s, 2H), 4.87-4.75 (m, 4H), 4.54˜4.49 (m, 2H), 3.90-3.88 (m, 2H), 3.67-3.45 (m, 20H), 3.39-3.32 (m, 4H), 3.31 (s, 6H), 3.17-3.05 (m, 4H), 1.41 (s, 1H). MS (m/z): 1189 [M+H]+.

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