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Methyl 4-(3,4-dimethoxybenzyloxy)-3-chlorobenzoate → 4-(3,4-Dimethoxybenzyloxy)-3-chlorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 4-(3,4-dimethoxybenzyloxy)-3-chlorobenzoate | HCID 57796893 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3,4-Dimethoxybenzyloxy)-3-chlorobenzoic acid | HCID 57796897 | 65% |
反応手順
A solution of 1A (600 mg, 1.78 mmol) in THF (30 mL) and MeOH (10 mL) was treated with a solution of LiOH monohydrate (375 mg, 8.93 mmol) in water (10 mL) at room temperature. The resulting suspension was stirred at room temperature for 18 hours. The reaction was concentrated to 30 mL, diluted with water (50 mL) and cooled to 0° C. The solution was brought to pH 5 with 1 N HCl and the resulting solid was collected by vacuum filtration. Residual water was removed from the solid material using azeotrope with toluene to afford 1B as a white solid (370 mg, 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07569725B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-db42c4e011a34661a55b8388fa8a5fa3 |
| 出典メモ | uspto-grants-2009_08 |