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Methylparaben → Methyl 4-((5-hydroxypentyl)oxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylparaben | HCID 7456 | — |
| 反応物 | 1,5-Pentanediol | HCID 8105 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 生成物 | Methyl 4-((5-hydroxypentyl)oxy)benzoate | HCID 65019122 | 68% |
反応手順
To a solution of methyl p-hydroxybenzoate (3.38 g), 1,5-pentanediol (2.30 g) and triphenylphosphine (5.96 g) in tetrahydrofuran (100 mL), diethylazodicarboxylate (2.2N toluene solution, 10 mL) was slowly added under ice cooling. The reaction mixture was stirred under ice cooling for 16 hours. The reaction mixture was concentrated and the residue was washed with n-hexane-ethyl acetate solution (n-hexane:ethyl acetate=1:1). The reaction mixture was concentrated and then purified by silica gel chromatography (n-hexane:ethyl acetate=64:36→45:55) to obtain the title compound (3.58 g) having the following physical properties.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822459B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-a3818d1f2e964e4abb49da749142a5ba |
| 出典メモ | uspto-grants-2014_09 |