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HRID 373340作成日:2026年10月25日

1,2-Dichloroethane → (+/-)-trans-3-bromo-6-cyano 3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1benzopyran

https://huagongshe.com/reaction/373340

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物trans-2,2-Dimethyl-3-bromo-6-cyanochroman-4-olHCID 6932483—
反応物(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyl chlorideHCID 15045107—
溶媒PyridineHCID 1049—
生成物(+/-)-trans-3-bromo-6-cyano 3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1benzopyranHCID 8674522993.1%

反応手順

To a mixture of 14.5 g of (±)-trans-3-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-4-hydroxy-2H-1-benzopyran, 60 ml of ethylene chloride and 1.6 ml of pyridine was added 5.5 g of (S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyl chloride under ice-cooling and was stirred for 1.5 hours under room temperature. The reaction mixture was washed with diluted hydrochloric acid once and 10% aqueous sodium chloride solution twice. The organic layer was separated, dried over magnesium sulfate and concentrated under reduced pressure to give 8.9 g of (±)-trans-3-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1-benzopyran as light yellow semicrystals.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05162553
出典データセットuspto-grants-1992_11
ORD IDord-d5225a4c078a401c8f15e00d25491bbb
出典メモuspto-grants-1992_11