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Hydrochloric Acid → 1-(2-amino-5-methoxyphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,5-Dimethyltetrazole | HCID 78825 | — |
| 反応物 | Methyl 2-amino-5-methoxybenzoate | HCID 13052275 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 1-(2-amino-5-methoxyphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanone | HCID 13474406 | — |
反応手順
A solution of butyl lithium in hexane (2.5M, 18.5 ml) was added to a stirred solution of 1,5-dimethyl-tetrazole (4.55 g) in dry tetrahydrofuran (100 ml) at 0°. After 30 minutes methyl 2-amino-5-methoxybenzoate (2.8 g) was added and stirring was continued for 3 hours. The reaction mixture was poured into water (200 ml), acidified with hydrochloric acid (5N) to pH 1, and extracted with dichloromethane (3×100 ml). The extract was dried over anhydrous magnesium sulphate and evaporated. The residue was recrystallised from industrial methylated spirit to give the novel compound 1-(2-amino-5-methoxyphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanone, m.p. 170°-172°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659718 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-047eaa02e81d440bb27f354bc50b6ce5 |
| 出典メモ | uspto-grants-1987_04 |