関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributylvinyltin | HCID 81998 | — |
| 反応物 | HCID 54481034 | HCID 54481034 | — |
| 触媒 | Bis(triphenylphosphine)palladium chloride | HCID 84124 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Diethylphosphonomethyloxy-5-vinylnitrobenzene | HCID 54101958 | — |
反応手順
A solution of 2-diethylphosphonomethyloxy-5-bromonitrobenzene (1 mmole, prepared as in Example 37, Step A) in DMF (5 mL) was treated with tributyl(vinyl)tin (1.2 mmole) and palladium bis(triphenylphosphine) dichloride (0.1 mmole), and the mixture was heated at 60° C. under nitrogen for 6 h. Evaporation and chromatography gave 2-diethylphosphonomethyloxy-5-vinylnitrobenzene as an oil which was subjected to Step B of Example 38, Step B of Example 36, and Step D of Example 34 to give 2-amino-7-ethyl-6-thiocyano-4-phosphonomethoxybenzothiazole (41.1). mp >167° C.(dec.). Anal. Calcd. for C11H12N3O4PS2: C:38.26; H:3.50; N:12.17. Found: C:37.87; H:3.47; N: 11.93.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06756360B1 |
|---|
| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-cb46442e978e4c5ea6ef46da9b68f99c |
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| 出典メモ | uspto-grants-2004_06 |
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