化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1-(3-Bromo-2-hydroxy-5-methylphenyl)ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Hydroxy-5-methylacetophenone | HCID 15068 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(3-Bromo-2-hydroxy-5-methylphenyl)ethan-1-one | HCID 11138918 | 48% |
反応手順
To a solution of 21.5 g (0.143 mol) of 28 in 40 mL of dry dichloromethane, 0.3 g of iron turnings was added. A solution of 10.7 mL (34.2 g, 0.215 mol) of bromine in 100 mL of dichloromethane was added dropwise with vigorous stirring for 20 min. This mixture was refluxed for 30 min, and then 300 mL of water was added. The organic layer was separated, and the aqueous layer was extracted with 2×100 mL of dichloromethane. The combined organic extracts were washed with saturated aqueous Na2SO3, dried over K2CO3, and then evaporated to dryness. Drying the residue in vacuum gave 15.7 g (48%) of 29 (bp 105-115° C./1 mm).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541521B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-9642d440da684f9394e48a7cdd79826a |
| 出典メモ | uspto-grants-2013_09 |