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HRID 3607作成日:2026年10月24日

Stannous chloride dihydrate → 6,7-Dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepin

https://huagongshe.com/ja/reaction/3607

反応式

関与物質

役割名称HCID仕込み量
反応物Stannous chloride dihydrateHCID 61436—
反応物6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepineHCID 21837030—
溶媒EthanolHCID 702—
溶媒TetrahydrofuranHCID 8028—
生成物6,7-Dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepinHCID 21836994102.3%

反応条件

温度55 °C

反応手順

To a solution of 0,50 g of 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 10 ml of ethyl alcohol and 2 ml of tetrahydrofuran is added 2.35 g of SnCl2.2H2O and the mixture stirred at 55° C. for 30 minutes. The solvents are evaporated in vacuo to a residue which is stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes and filtered through diatomaceous earth. The filter pad is washed with 2×10 ml of ethyl acetate and the combined extracts washed with brine, dried (Na2SO4) and evaporated in vacuo to give 0.47 g of solid residue which is triturated with ether-hexane to give 0.43 g of light yellow crystalline solid. MS(CI): 338 (M+H, Cl35) 340 (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-5d66cdab1c794ab784689ff5a3d4e879
出典メモuspto-grants-1998_03