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Tributylphosphine → Ethyl[2-methyl-4-(2-thien-2-ylethoxy)phenoxy]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | 2-Thiopheneethanol | HCID 79400 | — |
| 反応物 | Ethyl (4-hydroxy-2-methylphenoxy)acetate | HCID 21986458 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl[2-methyl-4-(2-thien-2-ylethoxy)phenoxy]acetate | HCID 21986308 | — |
反応手順
A solution of ethyl(4-hydroxy-2-methylphenoxy)acetate (intermediate 7, 1.05 g) and 2-(2-thienyl)ethanol (0.64 g) in dry tetrahydrofuran was treated with tri-n-butyl phosphine (1.2 g) and azodicarbonyldimorpholide (1.53 g) and the mixture stirred at ambient temperature for 3 days. The reaction mixture was concentrated and the residue partitioned between ethyl acetate and water. The organic layer was collected, dried over sodium sulfate, concentrated and the residue purified by SPE (Si cartridge) eluting with cyclohexane:ethyl acetate (20:1) to give the title compound as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091237B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ae8f35505a5f42f7845c7a23a233be40 |
| 出典メモ | uspto-grants-2006_08 |