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Water → methyl N-[(4-bromophenyl)sulfonyl]-L-valinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Methyl valinate hydrochloride | HCID 111190 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | methyl N-[(4-bromophenyl)sulfonyl]-L-valinate | HCID 47337186 | 84.5% |
反応手順
To a suspension of methyl valinate hydrochloride (10.0 g, 59.7 mmol) and sodium carbonate (15.8 g, 149 mmol) in acetone (200 ml)-water (100 mL) was added 4-bromobenzenesulfonyl chloride (12.7 g, 49.7 mmol) at 0° C., and the mixture was stirred at room temperature for 12 hr after addition. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate, washed with 0.1N hydrochloric acid, water and saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from hexane-ethyl acetate to give the title compound as a white powder (14.7 g, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07915267B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-18a2087bacef4f858c652956d4472523 |
| 出典メモ | uspto-grants-2011_03 |