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HRID 373736作成日:2026年10月26日

Acetic Acid → Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate

https://huagongshe.com/reaction/373736

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物WaterHCID 962—
反応物AcetonitrileHCID 6342—
反応物5-NitroisoquinolineHCID 69085—
反応物Tris(dimethylamino)sulfonium difluorotrimethylsilicateHCID 9795567—
溶媒HexaneHCID 8058—
生成物Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetateHCID 13507926—

反応手順

A flame dried 50 mL flask fitted with an addition funnel was charged with 0.872 g (500 mmol) of 5-nitroisoquinoline and 0.95 mL (5.1 mmol) of MTS. An acetonitrile solution of 1.40 g (5.09 mmol) of TASF was slowly added to the reaction mixture in 15 min at -78° C. The mixture was stirred for 22 h at that temperature. One mL of acetic acid in 5 mL of hexane was added, and reaction was warmed to room temperature. After 30 min, 40 mL of water was added. The solid which precipitated out was collected and analyzed. The product yield was 0.972 g (74%). The product material was analyzed by infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05164499
出典データセットuspto-grants-1992_11
ORD IDord-02f61dd96e9b44fa8d5cc71fd42e8da8
出典メモuspto-grants-1992_11