化工社化工社 化学情報印刷レポート · 研究参考用
Water → (3-Bromo-2-hydroxy-5-methylphenyl)(phenyl)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2-Hydroxy-5-methylbenzophenone | HCID 73851 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-Bromo-2-hydroxy-5-methylphenyl)(phenyl)methanone | HCID 12925474 | 86.2% |
反応手順
To a solution of 116 g (0.55 mol) of 32 in 200 mL of dry dichloromethane 1.5 g of iron turnings was added, and then a solution of 41.4 mL (136 g, 0.83 mol) of bromine in 500 mL of dichloromethane was added dropwise with vigorous stirring for 20 min. This mixture was refluxed for 30 min, and then 1200 mL of water was added. The organic layer was separated, and the aqueous layer was extracted with 2×300 mL of dichloromethane. The combined organic extract was washed by saturated aqueous Na2SO3, dried over K2CO3, and then evaporated to dryness. Drying the residue in vacuum gave 138 g (86%) of 33 (bp 165-172° 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-d284b72bcb284240b78ada4f1e65bc83 |
| 出典メモ | uspto-grants-2013_09 |