Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 18406943 | HCID 18406943 | — |
| Product | HCID 18406934 | HCID 18406934 | — |
Reaction Steps
1-(2,2-Difluoroethyl)-1H-[1,2,4]triazole (4.0 g, 0.030 mol) was heated at reflux in 37% aqueous formaldehyde for 2 days. The solution was allowed to cool to room temperature and was washed with dichloromethane (3×50 ml). The solution was then saturated with sodium chloride, and washed again with dichloromethane (3×50 ml). The combined organic washings were dried over magnesium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel, eluting with 0 to 7.5% methanol in dichloromethane, yielding [2-(2,2-difluoroethyl)-2H-[1,2,4]triazol-3-yl]methanol as a solid (2.4 g). Data for the title compound: 1H NMR (250 MHz, CDCl3) δ 4.65 (2H, td, J=13.2, 4.3 Hz), 4.83 (2H, s), 6.17 (1H, tt, J=55.2,4.3 Hz), 7.86 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06476030B1 |
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| Source dataset | uspto-grants-2002_11 |
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| ORD ID | ord-28bb9101dfd04af2a9eb2562ff93a869 |
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| Source note | uspto-grants-2002_11 |
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