化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-(t-Butyldimethylsilyloxymethyl)phenyl 2-(acetyloxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Acetoxybenzoyl chloride | HCID 79668 | — |
| 反応物 | 3-((((1,1-Dimethylethyl)dimethylsilyl)oxy)methyl)phenol | HCID 14940556 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(t-Butyldimethylsilyloxymethyl)phenyl 2-(acetyloxy)benzoate | HCID 12071054 | 100% |
反応手順
To a solution of Compound 3 in Et2O (120 ml) were added acetylsalicyloyl chloride (Compound 4) (5.9 g, 0.028 mol) and triethylamine (Et3N) (6.6 ml, 0.047 mol) in sequence at RT. The reaction mixture was stirred at RT under argon for 3 days. The reaction mixture was diluted with EtOAc (100 ml) and washed with aqueous saturated NaHCO3 (3×100 ml), brine (1×100 ml), and dried over anhydrous Na2SO4. The crude product obtained upon concentration was purified by column chromatography (elution solvent: 5% EtOAc in hexanes) to produce 9.4 g of Compound 5 in 100% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06538033B2 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-e698fe58e16d4fa2a1f2009aa22ff3b1 |
| 出典メモ | uspto-grants-2003_03 |