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Putrescine → N,N'-bis(mesitylenesulfonyl)putrescine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Putrescine | HCID 1045 | — |
| 反応物 | 2-Mesitylenesulfonyl chloride | HCID 13046 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | N,N'-bis(mesitylenesulfonyl)putrescine | HCID 10434030 | 90% |
反応手順
2-Mesitylenesulfonyl chloride (54.40 g, 0.249 mol) in CH2Cl2 (300 ml) was added to 1,4-diaminobutane (11.34 g, 0.129 mol) in 1 N NaOH (300 ml) at 0° C., and the biphasic mixture was stirred for 24 hours at room temperature. Organic solvent was evaporated and 2.4 N HCl (250 ml) was added to the combined portions. Solid was filtered, washed with water (250 ml) and recrystallized from aqueous ethanol to give 50.46 g (90%) of (1) as needles: mp 156.5-157.5° C.; NMR (CDCl3/TMS) δ 1.36-1.60 (m, 4H), 2.27 (s, 6H), 2.57 (s, 12H), 2.69-2.96 (m, 4H), 4.65 (t, 2H, J=6), 6.89 (s, 4H). Anal. calcd. for C22H32N2O4S2: C—58.38, H—7.13, N—6.19. Found: C—58.31, H—7.19, N—6.14.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094808B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-1867737373ad4bb48701270e5edc5939 |
| 出典メモ | uspto-grants-2006_08 |