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Triethylamine → Bis-[(2-triethylsilyl-4-furyl)methyl]oxalate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 4-Hydroxymethyl-2-triethylsilylfuran | HCID 15037035 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Bis-[(2-triethylsilyl-4-furyl)methyl]oxalate | HCID 15037121 | — |
反応手順
Oxalyl chloride (0.59 ml, 6.79 mmol) was added dropwise to a solution of 4-hydroxymethyl-2-triethylsilylfuran (Compound 1, 1.2 g, 5.66 mmol) and triethylamine (0.95 ml, 6.79 mmol) in dichloromethane (10 ml) at 0°. After 10 minutes, the reaction mixture was quenched with ice. Extraction (dichloromethane) and evaporation of the dried (magnesium sulfate) extracts gave an oil, which was purified by flash chromatography on silica using 5% ethyl ether/hexane. Fractions with Rf of about 0.17 gave, after evaporation the title oxalate ester as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05298633 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-f8016cc81bfd41548b2e81d770fabd5f |
| 出典メモ | uspto-grants-1994_03 |