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Potassium Carbonate → 3-(3-Methyl-benzyloxy)-phthalic acid dimethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | m-Xylyl bromide | HCID 12099 | — |
| 反応物 | Dimethyl 3-hydroxyphthalate | HCID 12223651 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3-(3-Methyl-benzyloxy)-phthalic acid dimethyl ester | HCID 66906352 | 114.3% |
反応手順
To a stirred suspension of 3-hydroxyphthalic acid dimethyl ester (1.4 g, 6.4 mmol) in acetone (30 mL) and potassium carbonate (2.7 g, 19.3 mmol) was added 1-bromomethyl-3-methyl-benzene (0.91 mL, 6.7 mmol) and refluxed overnight. The solvent was evaporated and the residue was partitioned between water (100 mL) and ethyl acetate (150 mL) and washed with water (2×100 mL). The combined organic phases was dried, concentrated and purified by flash column chromatography (EtOAc/Hexane) to give 3-(3-methyl-benzyloxy)-phthalic acid dimethyl ester (2.3 g, 115% crude yield). The product was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181216B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-3695141934754cf1a8365eb46d83cb2c |
| 出典メモ | uspto-grants-2015_11 |