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HRID 2940作成日:2026年10月24日

Water → 5-(3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methylene-N-methyl-4-thiazolidinone

https://huagongshe.com/ja/reaction/2940

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物TributylstannaneHCID 5948—
反応物AzobisisobutyronitrileHCID 6547—
反応物5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-3-methyl-2-thioxo-4-thiazolidinoneHCID 54389601—
溶媒TolueneHCID 1140—
生成物5-(3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methylene-N-methyl-4-thiazolidinoneHCID 13000171%

反応手順

The title compound was prepared in 71% yield from 10.31 g of the thione of Example 9 upon heating with 38.15 ml of tri-n-butyl tin hydride and 1.16 g of azobisisobutyronitrile (AIBN) in 142 ml of toluene at reflux temperature for one hour. The product was isolated by adding water to the cooled reaction mixture, separating the layers, washing the organic layer with 1N hydrochloric acid and a saturated sodium chloride solution, drying over magnesium sulfate, concentrating in vacuo, and purifying the residue by chromatography over silica gel eluting with a 10-50% hexane in ethyl acetate gradient. The purified product had a melting point of 142°-144° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05731336
出典データセットuspto-grants-1998_03
ORD IDord-867855b5cbc343afbf6e7d8206f20441
出典メモuspto-grants-1998_03