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Methanol → Methyl 3-bromothiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3-Bromothiophene-2-carboxylic acid | HCID 2739688 | — |
| 生成物 | Methyl 3-bromothiophene-2-carboxylate | HCID 2740074 | — |
反応手順
3-Bromothiophene-2-carboxylic acid (5.0 g, 24 mmol, 1 eq.) was dissolved in MeOH (100 mL) and the mixture was degassed and purged with nitrogen (2×). SOCl2 (15 mL, 0.2 mol, 8.3 eq.) was added dropwise and the resulting mixture was stirred overnight at room temperature. The mixture was then concentrated and DCM (150 mL) was added. Saturated NaHCO3 (20 mL) was added, and the resulting mixture was stirred at room temperature for 15 minutes. The organic layer was washed with saturated NaHCO3 (20 mL), water (20 mL), and saturated aqueous NaCl (20 mL), then dried over Na2SO4, filtered and concentrated to yield 3-bromothiophene-2-carboxylic acid methyl ester (4.0 g) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530663B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-80167fa325ac4c73b8b6b32d36edcb90 |
| 出典メモ | uspto-grants-2013_09 |