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Sulfuric Acid → 1-(1,1-dimethylethyl)-5-(2-methoxyphenyl)-2H-tetrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 5-(2-Methoxyphenyl)-1H-tetrazole | HCID 858908 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(1,1-dimethylethyl)-5-(2-methoxyphenyl)-2H-tetrazole | HCID 19371911 | 35.5% |
反応手順
A mixture of 5-(2-methoxyphenyl)-2H-tetrazole (0.83 g, 4.71 mmol), 2-methyl-2-propanol (0.7 g, 9.4 mmol), and sulfuric acid (0.24 g, 2.4 mmol) in 4.6 mL of TFA was stirred under nitrogen at room temperature for 16 hours. The reaction mixture then was diluted with ethyl acetate, poured into 2M potassium hydroxide, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate and concentrated. Purification of the residue by column chromatography on silica gel (elution: 10% ethyl acetate/hexane) gave 1-(1,1-dimethylethyl)-5-(2-methoxyphenyl)-2H-tetrazole (0.5102 g, 1.67 mmol), as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05468867 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-c15cc2766e114b60bb4f63376968896d |
| 出典メモ | uspto-grants-1995_11 |