化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Bicarbonate → Methyl 2-hydroxy-6-methoxymethylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 2-bromomethyl-6-(tert-butyldimethylsilyloxy)benzoate | HCID 25170261 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-hydroxy-6-methoxymethylbenzoate | HCID 89704969 | — |
反応手順
A solution of methyl 2-bromomethyl-6-(tert-butyldimethylsilyloxy)benzoate (Intermediate 12, 4.26 g) in methanol (63 mL) was stirred and heated at reflux overnight. After cooling, the mixture was basified by addition of solid sodium bicarbonate and then evaporated to dryness. The residue was triturated with DCM and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-25% to give methyl 2-hydroxy-6-methoxymethylbenzoate (1.46 g) as a white crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440943B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-a27c6335f7d34fb3be4947c9a70e0309 |
| 出典メモ | uspto-grants-2016_09 |