Acetic Acid Mixture with Hydrobromic Acid → HCID 21930359、化合物
反応式
[F:1][C:2]1[CH:11]=[CH:10][C:9]([O:12]C)=[CH:8][C:3]=1[CH2:4][N:5]([CH3:7])[CH3:6].[BrH:14].C(O)(=O)C>>[BrH:14].[CH3:7][N:5]([CH2:4][C:3]1[CH:8]=[C:9]([OH:12])[CH:10]=[CH:11][C:2]=1[F:1])[CH3:6]参加物
3
実験手順
(2-Fluoro-5-methoxybenzyl)-dimethylamine (1.51 g, 8.24 mmol) was heated to reflux in 30% hydrogen bromide/acetic acid (10 mL) for 17 h. The cooled reaction mixture was triturated and decanted with successive portions of diethyl ether (4×), then triturated with diethyl ether overnight. The solid was collected by filtration, washed with ether and dried to give 3-dimethylaminomethyl-4-fluorophenol hydrobromide (1.43 g, 69%) as a tan solid.
後処理
- customThe cooled reaction mixture
- customwas triturated
- customdecanted with successive portions of diethyl ether (4×)
- customtriturated with diethyl ether overnight
- filtrationThe solid was collected by filtration
- washwashed with ether
- customdried
出典と根拠
- ORDレコード
- ord-5f3e07de12344364b555900f61e33207
- 出典データセット
- uspto-grants-2007_10
- 特許番号
- US07276528B2
反応ノート
読み込み中…