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Methyl morpholine oxide → 6-chloro-N-(2,3-dihydroxypropyl)-N-phenylpyridine-3-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl morpholine oxide | HCID 82029 | — |
| 反応物 | Tetrahydrofuran hexane | HCID 21883165 | — |
| 反応物 | 6-chloro-N-phenyl-N-(prop-2-en-1-yl)pyridine-3-sulfonamide | HCID 24419482 | — |
| 触媒 | Osmium Tetroxide | HCID 30318 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 6-chloro-N-(2,3-dihydroxypropyl)-N-phenylpyridine-3-sulfonamide | HCID 86659756 | 80% |
反応手順
To a solution of 1.3 g (4.2 mmol) of 6-chloro-N-phenyl-N-(prop-2-en-1-yl)pyridine-3-sulfonamide in 17 mL of a mixture (1/1) of tBuOH and water are added, at room temperature, 1.37 g (11.7 mmol) of NMO and 0.52 mL (0.04 mmol) of 2.5% OsO4 in tBuOH. Stirring is continued for 12 hours. The medium is then diluted with 200 mL of water and extracted with Et2O (2×100 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. 1.14 g of 6-chloro-N-(2,3-dihydroxypropyl)-N-phenylpyridine-3-sulfonamide are obtained in the form of an oil, which is used without further purification in the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541455B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-4e96f7796f8746948ad806fa4b810484 |
| 出典メモ | uspto-grants-2013_09 |