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HRID 1576017作成日:2026年10月27日

Hydroquinone → 3-(4-Chlorophenyl)-7-[(4-chlorophenyl)methylene]-2,3,3a,4,6,7-hexahydro-2-propylthiopyrano[4,3-c]pyrazole

https://huagongshe.com/reaction/1576017

反応式

関与物質

役割名称HCID仕込み量
反応物HydroquinoneHCID 785—
反応物Hydrazine, propyl-HCID 42007—
反応物4H-Thiopyran-4-one, 3,5-bis[(4-chlorophenyl)methylene]tetrahydro-HCID 382469—
溶媒1,1-DichloroethaneHCID 6365—
生成物3-(4-Chlorophenyl)-7-[(4-chlorophenyl)methylene]-2,3,3a,4,6,7-hexahydro-2-propylthiopyrano[4,3-c]pyrazoleHCID 5365048940.4%

反応手順

A mixture of 6.0g of tetrahydro-3,5-bis-[(4-chlorophenyl)methylene]-4H-thiopyran-4-one, 1.3g of n-propyl hydrazine, and 100mg of hydroquinone in 100ml of dichloroethane is heated at reflux temperature for 2.5 hours and allowed to cool to room temperature. The reaction mixture is washed with dilute hydrochloric acid and water, and then dried over calcium chloride. After the solvent is removed in vacuo, the residue is chromatographed on a dry packed neutral alumina column (Activity I). The fractions eluted with 0-5% ethyl acetate/hexane are combined and crystallized from acetone/acetonitrile to give 2.8g of the title compound, melting point 118°-122°C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US03979381
出典データセットuspto-grants-1976_09
ORD IDord-b7b880a812034aebbe379598b6672279
出典メモuspto-grants-1976_09