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Methylparaben → Methyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylparaben | HCID 7456 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | N-(2-Hydroxyethyl)phthalimide | HCID 77499 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)benzoate | HCID 7679064 | — |
反応手順
A solution of N-(2-hydroxyethyl)phthalimide (Aldrich, 19-1, 6.36 g, 33 mmol) and DEAD (5.7 mL, 36 mmol) in 25 mL THF and 10 mL DMF was added to a solution of methyl 4-hydroxybenzoate (1-2, 5.00 g, 33 mmol) and Ph3P (9.53 g, 36 mmol) in 100 mL THF during 1 h. After an additional hour the reaction was diluted with ether, washed twice with water, then 1N NaOH and brine, dried (MgSO4), filtered and concentrated. Flash chromatography (silica gel, CH2Cl2) provided 19-2 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929120 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-38fe269c9aa64d9ca0e14a938a912982 |
| 出典メモ | uspto-grants-1999_07 |