Bromine → HCID 178432761, 화합물
반응식
[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]=1참가 물질
4
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-60b0e6ae961a46aeac9dc2d56954058e
- 출처 데이터셋
- uspto-grants-1984_06
- 특허 번호
- US04452987
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