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HRID 430656作成日:2026年10月25日

Phthalimide → 5-(4-Nitrophenyl)-8-(phthalimidomethyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine

https://huagongshe.com/reaction/430656

反応式

関与物質

役割名称HCID仕込み量
反応物PhthalimideHCID 6809—
反応物TriphenylphosphineHCID 11776—
反応物ethyl N-ethoxycarbonyliminocarbamateHCID 220568—
反応物8-Hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepineHCID 18183191—
溶媒TetrahydrofuranHCID 8028—
生成物5-(4-Nitrophenyl)-8-(phthalimidomethyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepineHCID 18183124—

反応手順

A solution of 1.25 ml (8.05 mmol) of diethyl azodicarboxylate in 7 ml of THF is added in drops to a stirred solution of 2.60 g (7.66 mmol) of 8-hydroxymethyl-5-(4-nitrophenyl)-9H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine (starting compound III.), 2.11 g (8.05 mmol) of triphenylphosphine and 1.18 g (8.05 mmol) of phthalimide in 130 ml of dry THF at room temperature. The mixture is stirred for 24 hours at this temperature. Then, the precipitated product is suctioned off and washed with ethanol. 2.87 g (80%) of the title compound, which can be further processed without further purification, is obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06323197B1
出典データセットuspto-grants-2001_11
ORD IDord-6429d3d3bc204717b1ac0026f57232c5
出典メモuspto-grants-2001_11