Hydrochloric Acid → 3-Chloro-o-cresol
反応式
Cl[C:2]12[O:8][CH:7]1[CH2:6][CH2:5][C:4](Cl)([Cl:9])[CH:3]2[CH3:11].Cl>CN(C=O)C>[Cl:9][C:4]1[C:3]([CH3:11])=[C:2]([OH:8])[CH:7]=[CH:6][CH:5]=1参加物
4
実験手順
2 g (9.28 mmol) of epoxide 2h in solution in 5 cm3 of anhydrous DMF were heated to reflux for 3 h. The solution was acidified (pH=1) with 3N HCl, extracted with ether (4×25 cm3), dried over MgSO4, filtered and evaporated down. The crude product obtained was purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95). 1.18 g of phenol 4e were obtained (macrobore GC purity>96%). The yield of compound 4e was 89%.
後処理
- temperatureto reflux for 3 h
- extractionextracted with ether (4×25 cm3)
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated down
- customThe crude product obtained
- customwas purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95)
出典と根拠
- ORDレコード
- ord-1ac2c1865d0a4e33a67f9b64d9f725a8
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424460
反応ノート
読み込み中…