化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → [4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Bromoform | HCID 5558 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 反応物 | 4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde | HCID 18359078 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | [4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid | HCID 18359186 | — |
反応手順
440 microliters of bromoform were added at −5° C. to a mixture of 4.26 mg of lithium bromide, 598 mg of potassium hydroxide and 5 ml of water and then, a solution of 825 mg of a 4-cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde (preparation given here-after) in 5 ml of dioxane was added dropwise. The mixture was stirred for 72 hours at 0° C. to −5° C. and was poured into a stirred mixture at 0° C. to −5° C. of 15 ml of ethyl acetate and 11 ml of hydrochloric acid. Extraction was carried out with ethyl acetate and the extracts were washed, dried and evaporated to dryness under reduced pressure. The oil obtained was used as is for the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06313305B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-b19382322eee470db0fdeb7fa38d1206 |
| 出典メモ | uspto-grants-2001_11 |