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Methylamine → 4-[1-Hydroxy-2-(methylamino)ethyl]benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 4-(Oxiran-2-yl)benzene-1-sulfonamide | HCID 22574283 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-[1-Hydroxy-2-(methylamino)ethyl]benzenesulfonamide | HCID 10192708 | 31.7% |
反応手順
To a solution of methyl amine (20 mL, 40 mmol, 2.0 M in methanol) was added 4-oxiran-2-ylbenzenesulfonamide (Preparation 49)(0.52 g, 2.6 mmol) at 0° C. The clear solution was warmed to room temperature and stirred overnight. The solvent and excess of methyl amine was evaporated to yield an oil. The crude oil was dissolved in methanol (5 mL), and stirred with resin (BioRad 50W×2, 1 g) for 4 hours. The resin was collected by filtration and washed with methanol (3×15 mL). The product on the resin was washed off with NH4OH/CH3OH (20 mL, 10% ammonium hydroxide aqueous solution (Aldrich, 29.4% NH3) in methanol). The solution was concentrated to dryness, and treated with high vacuum to give the title compound (0.19 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852731B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-bfbe96447d564e3bb7f88344810de5d6 |
| 出典メモ | uspto-grants-2005_02 |