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HRID 481469作成日:2026年10月26日

Sulfuric Acid → HCID 178520209、化合物

https://huagongshe.com/reaction/481469

反応式

関与物質

役割名称HCID仕込み量
反応物Sulfuric AcidHCID 1118—
反応物alpha-(1-Chlorocyclopropyl)-alpha-((2-chlorophenyl)methyl)-1H-1,2,4-triazole-1-ethanolHCID 119361—
反応物SulfurHCID 5362487—
反応物ButyllithiumHCID 178418339—
溶媒TetrahydrofuranHCID 8028—
溶媒HexaneHCID 8058—
生成物HCID 178520209HCID 17852020993%

反応条件

温度0 °C

反応手順

A mixture of 3.12 g (10 mmol) of 2-(1-chloro-cyclopropyl)-1-(2-chlorophenyl)-3-(1,2,4-triazol-1-yl)-propan-2-ol and 45 ml of absolute tetrahydrofuran is treated at 20° C. with 8.4 ml (21 mmol) of n-butyl-lithium in hexane, and the mixture is stirred at 0° C. for 30 minutes. The reaction mixture is then cooled to -70° C., 0.32 g (10 mmol) of sulphur powder are added, and the mixture is stirred for 30 minutes at -70° C. It is heated to -10° C., and treated with ice-water and brought to a pH of 5 by adding dilute sulphuric acid. The mixture is extracted repeatedly using ethyl acetate, and the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. In this manner, 3.2 g (93% of theory) of 2-(1-chloro-cyclopropyl)-1-(2-chlorophenyl)-3-(5-mercapto-1,2,4-triazol-1-yl)-propan-2-ol are obtained in the form of a solid which, after recrystallization, melts at 138°-139° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05789430
出典データセットuspto-grants-1998_08
ORD IDord-28423d9f0c2c4de4ba935d927efcac61
出典メモuspto-grants-1998_08