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Water → 3-Bromo-2,5-dimethoxybenzyl Alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 3-Bromo-2,5-dimethoxybenzaldehyde | HCID 931096 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Bromo-2,5-dimethoxybenzyl Alcohol | HCID 10192777 | 100% |
反応手順
A solution of 8.27 gm (33.75 mmol) of 3-bromo-2,5-dimethoxy benzaldehyde* in 40 ml THF and 20 ml water was cooled to 10° C. and treated portionwise with 3.83 gm (101.2 mmol) NaBH4. Stirring was maintained at ambient temperature until tlc analysis (silica gel; 1:4 ethyl acetate:hexane) indicated the absence of starting aldehyde. After 30 minutes the solvent was removed in vacuo and the residue was portioned between ethyl acetate and water. After washing with brine and drying (Na2SO4), the ethyl acetate extract was concentrated in vacuo to yield 8.34 gm (99%) of a white solid, mp 59°-60° C.; tlc (cited), Rf 0.12.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05807897 |
| 出典データセット | uspto-grants-1998_09 |
| ORD ID | ord-6abe74e3c66a411596eb4c01c542510a |
| 出典メモ | uspto-grants-1998_09 |