Carbon tetrabromide → HCID 20076910, 화합물
반응식
[C:1]([Br:5])(Br)(Br)[Br:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH:25]1[CH:29]=[CH:28][N:27]=[C:26]1[CH:30]=O>C(Cl)Cl>[Br:2][C:1]([Br:5])=[CH:30][C:26]1[NH:25][CH:29]=[CH:28][N:27]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
Mix carbon tetrabromide (49.8 g, 150 mmol) and methylene chloride (75 mL) and cool to 0° C. Add, by dropwise addition, a solution of triphenylphosphine (78.6 g, 300 mmol) in methylene chloride (75 mL). Stir at 0° C. for 30 minutes. Add, by dropwise addition, a solution of 2-imidazole-carboxaldehyde (7.57 g, 78.8 mmol) in methylene chloride (75 mL). Remove the cooling bath and stir at room temperature until the reaction is complete. Pour onto ethyl ether and water, separate the organic layer and dry (MgSO4). Filter and evaporate the solvent in vacuo. Purify by silica gel chromatography to yield the title compound.
후처리
- additionAdd, by dropwise addition
- additionAdd, by dropwise addition
- customRemove the cooling bath
- stirringstir at room temperature until the reaction
- additionPour onto ethyl ether and water
- customseparate the organic layer
- dry with materialdry (MgSO4)
- filtrationFilter
- customevaporate the solvent in vacuo
- customPurify by silica gel chromatography
출처 및 근거
- ORD 기록
- ord-aff6823a6cdf4ba9812c328ef6a8f662
- 출처 데이터셋
- uspto-grants-1993_06
- 특허 번호
- US05223518
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