関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | HCID 178482013 | HCID 178482013 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-diethyl-4-(1-methyl-1,2,3,4-tetrazol-5-yl)thio-butyramide | HCID 21153948 | 57.9% |
反応手順
3-(1-Methyl-1,2,3,4-tetrazol-5-yl)methylthiopropionic acid (2 g) is dissolved in tetrahydrofuran (50 ml), and thereto is added triethylamine (1.1 g). To the mixture is added dropwise with stirring isobutyl chloroformate (1.5 g) under ice-cooling, and the mixture is stirred at room temperature for 30 minutes. To the mixture is added dropwise with stirring diethylamine (0.9 g) at the same temperature, and the mixture is further stirred for 3 hours. After distilling off the solvent, the resulting residue is subjected to column chromatography (Kieselgel 60, made by Merck & Co., eluting solvent, chloroform:methanol=50:1, V/V) to isolate N,N-diethyl-3-(1-methyl-1,2,3,4-tetrazol-5-yl)methylthio-propionamide (1.5 g), colorless liquid, nD25 =1.5200.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04766120 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-20931139bee64cab9abe141841eacc96 |
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| 出典メモ | uspto-grants-1988_08 |
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