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Triphenylphosphine → 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 反応物 | 4-(3,3-Dichloro-2-propenyloxy)-2,6-dichlorophenol | HCID 11346738 | — |
| 反応物 | 4-(2,2-Diethoxyethoxy)butanol | HCID 18430111 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene | HCID 18429393 | 92.1% |
反応手順
To a mixture of 2.30 g of 4-(2,2-diethoxyethoxy)butanol, 2.94 g of 2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenol, 2.94 g of triphenylphosphine, and 30 ml of tetrahydrofuran was slowly added dropwise 2.48 g of diisopropylazodicarboxylate with stirring in a stream of nitrogen gas under ice cooling. After stirring at room temperature for 24 hours, the reaction mixture was concentrated to give a residue. This residue was subjected to silica gel chromatography, which afforded 4.48 g (yield, 73%) of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06448444B1 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-11a63c19d8ce410f821be956da910c78 |
| 出典メモ | uspto-grants-2002_09 |