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HRID 3606作成日:2026年10月23日

Triethylamine → 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine

https://huagongshe.com/ja/reaction/3606

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, 2-chloro-4-nitro-HCID 81522—
反応物6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepineHCID 12359341—
溶媒DichloromethaneHCID 6344—
生成物6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepineHCID 21837030105.6%

反応手順

To a solution of 0.28 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 6 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.50 g of 2-chloro-4-nitrobenzoyl chloride in 0.5 ml of methylene chloride. The reaction mixture is stirred at room temperature for 1 hour then quenched with 5 ml of saturated NaHCO3. The methylene chloride is evaporated in vacuo and the residue is diluted with 5 ml of water and extracted with 20 ml of ethyl acetate. The organic layer is separated washed with saturated NaHCO3 and brine, dried with Na2SO4 and evaporated in vacuo to give 0.59 g of a yellow foam which is triturated with ether-hexanes to give 0.56 g of the desired product as off-white solid. MS(CI): 368(M+H)(Cl35) 370 (M+H) (Cl37)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05733905
出典データセットuspto-grants-1998_03
ORD IDord-fa4012fada9d450bb1c4694877c81d19
出典メモuspto-grants-1998_03