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HRID 1638807作成日:2026年10月27日

Triethylamine → 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine

https://huagongshe.com/reaction/1638807

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Benzoyl chloride, 3,4,5-trimethoxy-HCID 78282—
反応物1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)piperazineHCID 10245231—
溶媒DichloromethaneHCID 6344—
生成物1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazineHCID 984922067.1%

反応手順

To a mixture of 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)piperazine (1.2 g), triethylamine (0.5 g) and methylene chloride (20 ml) is added dropwise, with stirring under ice-cooling, a solution of 3,4,5-trimethoxybenzoyl chloride (1.0 g) in methylene chloride (25 ml). The reaction mixture is stirred for one hour at room temperature. The reaction mixture is pourd into ice-water (100 ml), and extracted with methylene chloride. The organic layer is washed with water, dried and concentrated under reduced pressure. The concentrate is crystallized from ethyl acetatehexane to give 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-(3,4,5-trimethoxybenzoyl)piperazine (1.3 g), as obtained in Example 62, as colorless prisms, m.p. 164°-165° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04880809
出典データセットuspto-grants-1989_11
ORD IDord-b66aa2bc1aaa43afab4486b296594c86
出典メモuspto-grants-1989_11