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HRID 323169作成日:2026年10月26日

Diethyl Ether → 4-(4'-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-ylcarbonyl)aminoprop-1-yl]phenyl]benzamide

https://huagongshe.com/reaction/323169

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl EtherHCID 3283—
反応物Sodium borohydrideHCID 4311764—
反応物4-(4'-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-yl)carbonylamino-(1-propyn-1-yl)]phenyl]benzamideHCID 70070182—
触媒Dichloronickel;hexahydrateHCID 11791229—
溶媒MethanolHCID 887—
溶媒TetrahydrofuranHCID 8028—
生成物4-(4'-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-ylcarbonyl)aminoprop-1-yl]phenyl]benzamideHCID 2201056229.8%

反応手順

To an ice cooled mixture of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-yl)carbonylamino-(1-propyn-1-yl)]phenyl]benzamide (250 mg) and nickel chloride hexahydrate (297 mg) in a mixture of tetrahydrofuran (5 ml) and methanol (5 ml) was added sodium borohydride in small portions and the mixture was stirred at the same temperature for 1 hour. The mixture was filtered through bed of Celite and the filtrate was evaporated in vacuo. The residue was dissolved in chloroform (20 ml) and washed with water and brine. The organic solution was dried over magnesium sulfate and the solvent was evaporated in vacuo to give a syrup. The residue was solidified with diethyl ether to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-[3-(4-methylpiperazin-1-ylcarbonyl)aminoprop-1-yl]phenyl]benzamide (75.0 mg) as a powder.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06211242B1
出典データセットuspto-grants-2001_04
ORD IDord-e9f4748e503148fcb5e4ea2d6bc5ad00
出典メモuspto-grants-2001_04