関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Isoamyl Nitrite | HCID 8053 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | (4-Iodo-2,5-Dimethylphenyl)Amine | HCID 4770984 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1-Acetyl-5-iodo-6-methylindazole | HCID 59339735 | 21% |
反応手順
Acetic acid anhydride (6.9 mL, 72 mmol) was added to a slurry of 2,5-dimethyl-4-iodoaniline (6.0 g, 24 mmol) and potassium acetate (2.4 g, 24 mmol) in benzene (50 mL). The mixture was heated to 80° C. and isopentylnitrit (4.8 mL, 36 mmol) was added during 20 min. The mixture was stirred at 80° C. overnight, then cooled and filtered. The filtrate was evaporated and purified by column chromatography (SiO2, dichloromethane). Product containing fractions were pooled and concentrated. The subtitle compound (1.5 g, 21%) was obtained as crystals from ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07728030B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-15ee512a6807457dac01a4e09db860ab |
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| 出典メモ | uspto-grants-2010_06 |
|---|
