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Acetic Acid → Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 5-Nitroisoquinoline | HCID 69085 | — |
| 反応物 | Tris(dimethylamino)sulfonium difluorotrimethylsilicate | HCID 9795567 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05164499 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-02f61dd96e9b44fa8d5cc71fd42e8da8 |
| 出典メモ | uspto-grants-1992_11 |