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HRID 362354作成日:2026年10月25日

Triethylamine → 10,11-Dihydro-10-(4-nitrobenzoyl)dibenz[b,f][1,4]thiazepine

https://huagongshe.com/reaction/362354

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物4-Nitrobenzoyl chlorideHCID 8502—
反応物10,11-Dihydrodibenzo(b,f)(1,4)thiazepineHCID 12310482—
触媒4-(Dimethylamino)pyridineHCID 14284—
溶媒DichloromethaneHCID 6344—
生成物10,11-Dihydro-10-(4-nitrobenzoyl)dibenz[b,f][1,4]thiazepineHCID 54570072112.6%

反応手順

To a solution of 1.6 g of 10,11-dihydrodibenz[b,f][1,4]thiazepine in 30 ml of dichloromethane is added 0.1 g of 4-(N,N-dimethylamino)pyridine, 4 ml of triethylamine and 1.0 g of 4-nitrobenzoyl chloride and the mixture is stirred for 16 hours. The mixture is poured into ice-water and extracted with 3×150 ml of dichloromethane. The combined organic extract is washed with water, 2N HCl, 2N Na2CO3, water and dried (MgSO4). The solvent is removed in vacuo and the product (2.6 g) purified by chromatography on silica is gel with hexane-ethyl acetate (4:1) as eluent to give 2.2 g of crystals, m.p. 147°-149° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05869483
出典データセットuspto-grants-1999_02
ORD IDord-be832396dc934b20a7511ec1baf80991
出典メモuspto-grants-1999_02