Bromine → HCID 178432761、化合物
反応式
[C:1]([C:4]1[NH:8][C:7]([CH3:9])=[N:6][C:5]=1[CH3:10])(=[O:3])[CH3:2].[Br:11]Br>Br>[CH3:9][C:7]1[NH:8][C:4]([C:1](=[O:3])[CH2:2][Br:11])=[C:5]([CH3:10])[N:6]=1参加物
4
実験手順
A solution of 1.0 g (7.24 mmol) of 5-acetyl-2,4-dimethylimidazole in 15 ml of concentrated hydrobromic acid was warmed to 50° and 1.16 g (7.25 mmol) of bromine was added dropwise over 1 minute. The mixture was then heated at 50°-60° for 1 hour. The mixture was concentrated and the solid residue was triturated with 30 ml of saturated sodium bicarbonate solution. The insoluble material was collected by filtration, washed with water, and dried in vacuo to give 1.12 g (71%) of 1-(2,4-dimethyl-5-imidazolyl)-2-bromoethanone as a white solid, mp 128°-132°. nmr (D6DMSO) (δ): 4.40 (s, 2H); 2.27 (s, 3H); 2.13 (s, 3H).
後処理
- temperatureThe mixture was then heated at 50°-60° for 1 hour
- concentrationThe mixture was concentrated
- customthe solid residue was triturated with 30 ml of saturated sodium bicarbonate solution
- filtrationThe insoluble material was collected by filtration
- washwashed with water
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-9806d77fa1e749568394e497949b047c
- 出典データセット
- uspto-grants-1983_02
- 特許番号
- US04374843
反応ノート
読み込み中…