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4-Methoxybenzenesulfonyl chloride → 4-methoxy-n-Decylsulfamoylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| 反応物 | Decylamine | HCID 8916 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-methoxy-n-Decylsulfamoylbenzene | HCID 5201369 | 66.9% |
反応手順
Commercially available 4-methoxybenzenesulfonylchloride (Aldrich; 25 g, 0.12 moles) is added portionwise to a solution of decylamine (Kodak; 19 g, 0.12 moles) in pyridine (75 mL). The heterogeneous reaction mixture is stirred overnight at room temperature and poured into dilute HCl/ice water (1.5 L). After stirring 30 minutes, the light orange solid is isolated by filtration, washed with water and air dried. Recrystallization from ethanol (Norite) affords 26.3 g (66% yield) of the desired product as golden platelets, mp 53°-54.5° C. NMR (CDCl3) d 0.8-0.95 (t, 3H's); 1.1-1.6 (m, 16H's); 2.8-3.0 (t, 2H's); 3.9 (s, 3H's); 6.95-7.0 (d, 2H's); 7.75-7.85 (d, 2H's).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05468587 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-35cc5ce59e954d9bae0a3b8762b75909 |
| 出典メモ | uspto-grants-1995_11 |