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Ethanol → (s)-1-Chloro-3-(4-methylsulfonyl-1-piperazinyl)-2-propanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | (+)-Epichlorohydrin | HCID 149428 | — |
| 反応物 | 1-Piperazinesulfonamide | HCID 11252198 | — |
| 生成物 | (s)-1-Chloro-3-(4-methylsulfonyl-1-piperazinyl)-2-propanol | HCID 44249051 | — |
反応手順
(S)-Epichlorohydrin (48.0 mL, 0.612 mol) was added to a stirred solution of piperazine sulfonamide (87.3 g, 0.532 mol) in ethanol (1.33 L) at room temperature. The reaction mixture was stirred for 18 h and the white solid precipitate which formed was collected by filtration and washed with ethanol to afford the title intermediate (107.76 g) as a white solid which was used without further purification. (m/z): [M+H]+ calcd for C8H17ClN2O3S, 257.07; found 257.2. 1H NMR (DMSO-d6): δ (ppm) 2.37 (dd, 1H), 2.45 (dd, 1H), 2.50-2.58 (m, 4H), 2.86 (s, 3H), 3.09 (m, 4H), 3.55 (dd, 1H), 3.65 (dd, 1H), 3.84 (m, 1H), 5.09 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07419989B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-9ec7ebc7c00949548bcf741cc7809e4a |
| 出典メモ | uspto-grants-2008_09 |