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Nitrogen → 1-(2-Hydroxymethyl-oxazol-4-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 反応物 | HCID 131730009 | HCID 131730009 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-Hydroxymethyl-oxazol-4-yl)ethanone | HCID 66928792 | — |
反応手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-[2-(tert-butyl-dimethyl-silanyloxymethyl)-oxazol-4-yl]-ethanone (192 mg, 0.75 mmol) in dry THF (5.0 mL) was treated at rt with TBAF (1.1 mL of a 1M solution in THF, 1.10 mmol). The reaction mixture was stirred at rt for 1.5 h. The mixture was then diluted with EA (10 mL), washed with brine (3×10 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. Purification of the residue by FC (1:1 to 2:1 EA-Hept) gave the title compound as a pale yellow solid. TLC: rf (EA)=0.37. LC-MS-conditions 02: tR=0.34 min, [M+H]+=142.46.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08580831B2 |
| 出典データセット | uspto-grants-2013_11 |
| ORD ID | ord-87d3444119514695a4c4478f0a9e2086 |
| 出典メモ | uspto-grants-2013_11 |