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HRID 988978作成日:2026年10月25日

1,2-Dichloroethane → (4-Azido-phenyl)-(7-methoxy-1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-methanone

https://huagongshe.com/reaction/988978

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物TetrahydrofuranHCID 8028—
反応物DiisopropylethylamineHCID 81531—
反応物2-Azidobenzoic acidHCID 5325560—
反応物7-Methoxy-2,3,4,5-tetrahydro-1h-3-benzazepineHCID 13853348—
触媒4-(Dimethylamino)pyridineHCID 14284—
生成物(4-Azido-phenyl)-(7-methoxy-1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-methanoneHCID 22250962—

反応手順

7-Methoxy-2,3,4,5-tetrahydro-1 H-benzo[d]azepine (1 equivalent) was dissolved in THF (0.1 M) along with azidobenzoic acid (1.5 equivalents), EDC (1.5 equivalents), DMAP (0.18 equivalents), and DIEA (1.5 equivalents). The reaction was stirred at room temperature overnight. The reaction was then washed with 10% citric acid, saturated sodium carbonate, and brine. The organic layer was then dried over sodium sulfate and the organic solvent removed under reduced pressure. The material was then purified via flash chromatography using 8% acetone/1% ammonia solution/petroleum spirit running solvent to give the title compound. (MH+) 323.2.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06638927B2
出典データセットuspto-grants-2003_10
ORD IDord-5ecdccf389194922a6805571a74f24b0
出典メモuspto-grants-2003_10