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Methylenetriphenylphosphorane → 6-Bromo-8-vinyl-2,2,4,4-tetramethyl-chroman
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylenetriphenylphosphorane | HCID 137960 | — |
| 反応物 | 6-Bromo-2,2,4,4-tetramethyl chroman-8-carbaldehyde | HCID 22568946 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 触媒 | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 6-Bromo-8-vinyl-2,2,4,4-tetramethyl-chroman | HCID 22568922 | 72% |
反応手順
A solution of methylidene triphenyl phosphorane [generated from methyl triphenylphosphonium bromide (7 g, 20 mmol) and (11.8 mL, 19 mmol) of a 1.6M solution of n-butyl lithium in hexanes] was added 6-bromo-2,2,4,4-tetramethyl chroman-8-carbaldehyde (Intermediate 30, 0.52 g, 1.75 mmol). After 1 h the reaction mixture was diluted with hexane, washed with brine (×1), dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to a clear oil which was subjected to flash column chromatography over silica gel (230-400 mesh) using 2% ethyl acetate in hexane as the eluent to afford the title compound as a clear oil (0.37 g, 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713647B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-a36b1875d1ba4772826b3056ecc53604 |
| 出典メモ | uspto-grants-2004_03 |