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2-Aminobenzyl alcohol → N-(2-(hydroxymethyl)phenyl)methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Aminobenzyl alcohol | HCID 21439 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | N-(2-(hydroxymethyl)phenyl)methanesulfonamide | HCID 22955815 | 53.8% |
反応手順
A solution of methane sulfonyl chloride (10.2 ml, 0.13 mol) in chloroform (100 mL) was added dropwise to a solution of (2-aminophenyl)methanol (15.0 g, 0.12 mol) in pyridine (100 mL) and chloroform (150 mL) under nitrogen over 1 h at 0° C. The reaction mixture was stirred for 12 h at ambient temperature and then washed with hydrochloric acid (2N, 200 ml×2). The organic phase was dried over anhydrous MgSO4 and concentrated. The residue was purified by flash column chromatography on silica gel (EtOAc/hexane=1:3) to afford N-[2-(hydroxymethyl)phenyl]methanesulfonamide (13.0 g, 53% yield) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434761B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-cc7c2c09648b42f9ab0908c369380260 |
| 出典メモ | uspto-grants-2016_09 |