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Sodium Hydroxide → Methyl 4-(2-chloropyrimidin-4-ylthio)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,4-Dichloropyrimidine | HCID 77531 | — |
| 反応物 | Methyl 4-sulfanylbenzoate | HCID 237573 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 4-(2-chloropyrimidin-4-ylthio)benzoate | HCID 86645567 | 97% |
反応手順
To a sodium hydroxide (2.38 g, 59 mmol) solution in methanol (50 mL) and water (5 mL), was added dropwise a solution of methyl 4-mercaptobenzoate (9.00 g, 54 mmol) in methanol (100 mL). The mixture was stirred at room temperature for 1 hour, to this was added methanol solution (100 mL) of 2,4-dichloropyrimidine (8.77 g, 59 mmol) over 5 minutes. The whole was stirred at room temperature for 16 hours. Methanol was removed in vacuo, and the residue was partitioned between ethyl acetate (200 mL) and water (100 mL). The organic layer was separated and dried (Na2SO4). Removal of the solvent in vacuo yielded the product (14.60 g, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846704B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-83b45eba4ee148e4b7259d52a21eb72b |
| 出典メモ | uspto-grants-2014_09 |