関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 1H-1,2,4-Triazole-1-ethanol | HCID 550925 | — |
| 生成物 | 2-(5-Hydroxymethyl-1,2,4-triazol-1-yl)ethanol | HCID 18314528 | 68% |
反応手順
A solution of 2-(1,2,4-triazol-1yl)ethanol (5.0 g, 44 mmol) in 38% w/v aqueous formaldehyde (25 ml) was stirred and heated at 135° C. in a sealed tube for 18 hours. Upon cooling the volatiles were removed in vacuo (azeotroping with ethanol). The residue was purified by chromatography on silica gel, eluting with 5→10→15% methanol-dichloromethane to give the title compound (4.3 g, 68%) as a thick oil. 1H NMR (360 MHz, d6-DMSO) δ 3.69-3.74 (2H, m), 4.24 (2H, t, J=5.7 Hz), 4.60 (2H, d, J=5.7 Hz), 4.96 (1H, t, J=5.3 Hz), 5.51 (1H, t, J=5.8 Hz), 7.84 (1H, s); MS (ES+) m/e 144 [MH]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06355798B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-b27575f832e7405897e6d72dd1866d46 |
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| 出典メモ | uspto-grants-2002_03 |
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