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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 diazene-1,2-dicarboxylate | HCID 75555 | — |
| 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 diisopropyl azodicarboxylate with stirring under ice cooling. After stirring at room temperature for 24 hours, the reaction mixture was concentrated. The residue was subjected to silica gel chromatography, which afforded 4.48 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene (yield, 73%), nD24.5 1.5165.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06140274 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-7b8ec5e7036342029bc2f0684bd4f2b8 |
| 出典メモ | uspto-grants-2000_10 |