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Hydrochloric Acid → 5-Bromo-6-methoxy-pyridine-3-sulfonic acid (2-hydroxy-1-hydroxymethyl-1-methyl-ethyl)-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 5-Bromo-6-chloro-N-(1,3-dihydroxy-2-methylpropan-2-yl)pyridine-3-sulfonamide | HCID 86607992 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Bromo-6-methoxy-pyridine-3-sulfonic acid (2-hydroxy-1-hydroxymethyl-1-methyl-ethyl)-amide | HCID 67000075 | 51% |
反応手順
To a solution of 5-Bromo-6-chloro-pyridine-3-sulfonic acid (2-hydroxy-1-hydroxymethyl-1-methyl-ethyl)-amide (550 mg, 2 mmol) in MeOH (5 mL) was added a solution of sodium methoxide (c=5.4 mol/L in MeOH, 10 mmol) at rt for 48 h. The reaction mixture was poured into a 1N solution of HCl and was extracted with 2 portions of EtOAc, dried over Na2SO4, filtered, concentrated, and purified by column chromatography (heptane/EtOAc, 1:1) to give the title compound (0.28 g, 51%) as a white solid. MS (ISN) 353.1 [(M−H)−], 355.1 [(M+2−H)−].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07446113B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-30860c4336d840f880a82da224816964 |
| 出典メモ | uspto-grants-2008_11 |