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 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-(5-Chloro-pyridin-2-yl)-5-isobutyrylamino-benzoic acid methyl ester | HCID 57851430 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(5-Chloro-pyridin-2-yl)-5-(5-isopropyl-tetrazol-1-yl)-benzoic acid methyl ester | HCID 57851604 | 90.1% |
反応手順
3-(5-Chloro-pyridin-2-yl)-5-isobutyrylamino-benzoic acid methyl ester (1.90 g, 5.71 mmol) was dissolved in acetonitrile, and NaN3 (3.71 g, 5.71 mmol) and SiCl4 (1.64 mL, 14.28 mmol) were added. The reaction mixture was stirred at 60° C. for 18 hours, then cooled and poured in to cold saturated aqueous NaHCO3. The resulting mixture was extracted with EtOAc, and the combined organic layers were dried (MgSO4), filtered and concentrated under reduced pressure to give 1.84 g of 3-(5-chloro-pyridin-2-yl)-5-(5-isopropyl-tetrazol-1-yl)-benzoic acid methyl ester, MS (M+H)=358.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841336B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-791513e75ff44e2d89be8018f7f5923e |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
