6-Bromo-3-benzofuranacetonitrile → HCID 57192363, 화합물
반응식
[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[C:6]([CH2:9][C:10]#[N:11])=[CH:7][O:8][C:4]=2[CH:3]=1>C1COCC1>[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[C:6]([CH2:9][CH2:10][NH2:11])=[CH:7][O:8][C:4]=2[CH:3]=1참가 물질
3
실험 절차
A solution of 11-6 (10.9 g, 0.0462 mol) in THF (100 mL) was cooled to 0° C. and treated dropwise with BH3 /THF solution (1Molar, 110.8 mL, 0.11 mol). The cold bath was removed and the reaction stirred overnight. MeOH was carefully added (20 mL) and the solvent removed under vacuum. The residue was dissolved in 50 mL MeOH and 400 mL MeOH saturated with HCl and heated to reflux for 3 hours. The volatile components were removed under vacuum and the residue was suspended in Et2O. A bright yellow solid percipitated and was collected and washed five times with Et2O, then dried under vacuum to give 11-7 as a tan solid.
후처리
- customThe cold bath was removed
- additionMeOH was carefully added (20 mL)
- customthe solvent removed under vacuum
- dissolutionThe residue was dissolved in 50 mL MeOH
- temperature400 mL MeOH saturated with HCl and heated
- temperatureto reflux for 3 hours
- customThe volatile components were removed under vacuum
- customA bright yellow solid percipitated and was collected
- washwashed five times with Et2O
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-a9fd2a6783df4b84b0c95c92aca448b9
- 출처 데이터셋
- uspto-grants-1998_12
- 특허 번호
- US05854245
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