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HRID 1359563作成日:2026年10月25日

Water → 8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

https://huagongshe.com/reaction/1359563

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium metaborateHCID 145326—
反応物8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepineHCID 10893077—
溶媒TetrahydrofuranHCID 8028—
生成物8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepineHCID 1818319178.4%

反応条件

温度20 °C

反応手順

2.5 g (7.41 mmol) of 8-formyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine (I, stage A) is suspended in THF:water=1:1 and mixed with 0.14 g (3.7 mmol) of sodium boranate while being stirred and cooled to 20° C. After 45 minutes of stirring, it is filtered and the crude product is precipitated from the filtrate with 130 ml of water. 2.35 g, which is recrystallized from a mixture of 6.3 ml of dimethylformamide and 1.3 ml of water, is obtained. 1.97 g (78%) of the title compound with a melting point of 175° C. (decomposition) is obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06600036B2
出典データセットuspto-grants-2003_07
ORD IDord-53cc19ebc4ab4e9983c0880dc0bc2169
出典メモuspto-grants-2003_07