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Trimethylsilylmethyl Azide → HCID 67496021、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilylmethyl Azide | HCID 150751 | — |
| 反応物 | ETHYL 3-(4-FLUOROPHENYL)PROPIOLATE | HCID 12027755 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | HCID 67496021 | HCID 67496021 | 41.2% |
反応手順
To a solution of (4-fluoro-phenyl)-propynoic acid ethyl ester (1.45 g, 7.55 mmol) in benzene (25 mL) was added azidomethyl-trimethyl-silane (1.17 g, 9.05 mmol) and the reaction mixture was refluxed under nitrogen for 72 h. A subsequent batch of azidomethyl-trimethyl-silane (0.29 g, 2.26 mmol) was added and refluxing was continued for 5 h. The mixture was then evaporated and purification by chromatography (silica, 0 to 50% ethyl acetate in heptane) afforded the title compound (1.0 g, 41%) as a yellow oil. MS: m/e=322.2 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08742097B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-9b8ceadd3ad94883a7a2cfa22d3e7a9e |
| 出典メモ | uspto-grants-2014_06 |