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2-Methoxyacetohydrazide → methyl 2-isopropyl-5-(5-(methoxymethyl)-4H-1,2,4-triazol-3-yl)-4-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methoxyacetohydrazide | HCID 2759532 | — |
| 反応物 | Methyl 5-(imino(methylthio)methyl)-2-isopropyl-4-methylbenzoate | HCID 68288919 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | methyl 2-isopropyl-5-(5-(methoxymethyl)-4H-1,2,4-triazol-3-yl)-4-methylbenzoate | HCID 178494710 | 27.4% |
反応手順
A solution of methyl 5-(imino(methylthio)methyl)-2-isopropyl-4-methylbenzoate (compound 196.5, 800 mg, 3.01 mmol, 1.00 equiv) and 2-methoxyacetohydrazide (compound 190.6, 1.90 g, 18.3 mmol, 5.00 equiv) in acetic acid (30 mL) was stirred for 2 h at 80° C. in an oil bath, then concentrated in vacuo. The residue was purified using silica gel column chromatography with ethyl acetate/petroleum ether (1:50-1:2) as eluent to yield 250 mg (27%) of methyl 2-isopropyl-5-(5-(methoxymethyl)-4H-1,2,4-triazol-3-yl)-4-methylbenzoate as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871790B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-7b5c7239c3c9404ebcb58f8f9ed19390 |
| 出典メモ | uspto-grants-2014_10 |