関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl morpholine oxide | HCID 82029 | — |
| 反応物 | 4,4,6-Trimethyl-2-vinyl-1,3,2-dioxaborinane | HCID 107310 | — |
| 反応物 | (2-Phenyl4bromobenzoyl)-methionine methyl ester | HCID 20622824 | — |
| 触媒 | Osmium Tetroxide | HCID 30318 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 4-Formyl-2-phenylbenzoyl methionine methyl ester | HCID 10571267 | — |
反応手順
A mixture of (2-phenyl-4-bromobenzoyl) methionine methyl ester (100 mmol), 4,4,6-trimethyl-2-vinyl-1,3,2-dioxaborinane (100 mmol), tetrakis(triphenylphosphine)palladium (0) (3 mmol) in toluene and 2 M sodium carbonate in water (100 mL) is heated at 80° C. until the starting methyl ester disappears. The resulting mixture is extracted with ether, and washed with water, brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue is then purified by column chromatography on silica gel. To a solution of the resulting vinyl compound in dioxane/water (4/1) is added osmium tetraoxide (0.03 equivalent), N-methylmorpholine N-oxide (3 equivalents), and the reaction is stirred at 25° C. until TLC analysis shows the reaction to be complete. The reaction mixture is extracted with ether, which is washed with water and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue is then purified by column chromatography on silica gel to afford the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06221865B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-be157c7f9f90487b94fc7114f8218bd8 |
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| 出典メモ | uspto-grants-2001_04 |
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