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Nitroethane → 3-Nitro-1-phenoxy-butan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitroethane | HCID 6587 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Phenoxyacetaldehyde | HCID 75033 | — |
| 反応物 | 2,8,9-Triisopropyl-2,5,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane | HCID 5148322 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 3-Nitro-1-phenoxy-butan-2-ol | HCID 15105308 | 81% |
反応手順
2-Phenoxyacetaldehyde (1.36 g, 10 mmol) was added to a suspension of anhydrous magnesium sulfate (2.65 g, 22 mmol) in nitroethane (7.0 mL) under an argon atmosphere. After 5 min a solution of 2,8,9-triisopropyl-2,5,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane (0.30 g, 1.0 mmol) in nitromethane (3.0 mL) was added. The mixture was vigorously stirred for 5 days at r.t., filtered through celite and concentrated. Purification by column chromatography (SiO2, dichloromethane/t-butyl methyl ether) gave the subtitle compound as an oil (1.7 g, 81%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728030B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-fe19162b385a4d96923b629a75311512 |
| 出典メモ | uspto-grants-2010_06 |