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Silicon tetrachloride → 4'-Methyl-5-(5-methyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Silicon tetrachloride | HCID 24816 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 5-Acetylamino-4'-methyl-biphenyl-3-carboxylic acid methyl ester | HCID 57851440 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4'-Methyl-5-(5-methyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester | HCID 57850931 | 85% |
反応手順
A mixture of tetrachlorosilane (10.07 mmol, 2 mL), NaN3 (30.21 mmol, 1.96 g) and 5-acetylamino-4′-methyl-biphenyl-3-carboxylic acid methyl ester (3.36 mmol, 950.9 mg) in 10 ml of dry acetonitrile was stirred at room temperature for 16 hours. The reaction mixture were poured into ice-cold aqueous Na2CO3 solution and extracted with ethyl acetate (100 mL). The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The resulting crude 4′-methyl-5-(5-methyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester was used for next step directly (880 mg, 85% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846945B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-f8c35c72991b4cd4ac2dd7d8cc91c7f0 |
| 出典メモ | uspto-grants-2014_09 |