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HRID 46874作成日:2026年10月25日

Sodium Carbonate → 8-[3-(1,3-dihydro-5-methyl-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one

https://huagongshe.com/reaction/46874

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物1-Phenyl-1,3,8-triazaspiro(4.5)decan-4-oneHCID 70556—
反応物1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one methanesulfonateHCID 86735356—
溶媒DimethylformamideHCID 6228—
生成物8-[3-(1,3-dihydro-5-methyl-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-oneHCID 2038562824%

反応条件

温度60 °C

反応手順

A mixture of 5.68 parts of 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one methanesulfonate, 4.62 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 3.7 parts of sodium carbonate and 45 parts of N,N-dimethylformamide is stirred for 1 hour at 60° C. The reaction mixture is cooled and poured onto water. The precipitated product is filtered off and purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from a mixture of N,N-dimethylformamide and water, yielding 2 parts (24%) of 8-[3-(1,3-dihydro-5-methyl-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one; mp. 255.5° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04175129
出典データセットuspto-grants-1979_11
ORD IDord-e0a9860d9ec8465a988c31ecbd382387
出典メモuspto-grants-1979_11