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 | 54% |
反応手順
4-(1-Methyl-1,2,3,4-tetrazol-5-yl)thio-butyric acid (2 g) is dissolved in dry tetrahydrofuran (30 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. The mixture is stirred at room temperature for 30 minutes. To the mixture is further added dropwise with stirring diethylamine (0.9 g) at room temperature, and the mixture is stirred for 2 hours. The mixture is concentrated under reduced pressure, and the resulting residue is purified by subjecting it to column chromatography (Kieselgel 60, made by Merck & Co.). By eluting with n-hexane-ethyl acetate (1:1), there is obtained N,N-diethyl-4-(1-methyl-1,2,3,4-tetrazol-5-yl)thio-butyramide (1.4 g), colorless liquid, nD17.5 =1.5227
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04663323 |
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| 出典データセット | uspto-grants-1987_05 |
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| ORD ID | ord-69463ce0d61e4188b54cdf080fab327d |
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| 出典メモ | uspto-grants-1987_05 |
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