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HRID 2390633作成日:2026年10月24日

p-Toluenesulfonic acid → N-(4-{4-amino-7-[(1E)-3-oxoprop-1-enyl]thieno[3,2-c]pyridin-3-yl}-2-methoxyphenyl)-1-methyl-1H-indole-2-carboxamide

https://huagongshe.com/ja/reaction/2390633

反応式

関与物質

役割名称HCID仕込み量
反応物p-Toluenesulfonic acidHCID 6101—
反応物n-(4-{4-Amino-7-[(1e)-3,3-diethoxy-1-propenyl]thieno[3,2-c]pyridin-3-yl}-2-methoxyphenyl)-1-methyl-1h-indole-2-carboxamideHCID 18450992—
溶媒AcetoneHCID 180—
溶媒WaterHCID 962—
生成物N-(4-{4-amino-7-[(1E)-3-oxoprop-1-enyl]thieno[3,2-c]pyridin-3-yl}-2-methoxyphenyl)-1-methyl-1H-indole-2-carboxamideHCID 1845105099.7%

反応手順

A mixture of Example 176B (90 mg, 0.16 mmol) in acetone (9 mL) and water (1 mL) was treated with p-toluenesulfonic acid (5 mg, 0.016 mmol) then stirred for 30 minutes. The solvent was evaporated under reduced pressure then the residue was partitioned between dichloromethane and water. The organic layer was concentrated and the residue was purified by flash chromatography on silica gel to provide the desired product (77 mg). 1H NMR (DMSO-d6, 400 MHz) δ 9.67 (d, 1H), 9.52 (s, 1H), 8.34 (s, 1H), 8.03 (d, 1H), 7.91 (d, 1H), 7.75 (s, 1H), 7.70 (d, 1H), 7.32 (m, 2H), 7.25 (s, 1H), 7.10 (m, 3H), 6.69 (m, 1H), 4.04 (s, 3H), 3.92 (s, 3H); MS m/e 483.3.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08273736B2
出典データセットuspto-grants-2012_09
ORD IDord-577d218145f3454fad7f01d836981c82
出典メモuspto-grants-2012_09