6-Bromo-3-benzofuranacetonitrile → HCID 57192363、化合物
反応式
[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]=1参加物
3
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-a9fd2a6783df4b84b0c95c92aca448b9
- 出典データセット
- uspto-grants-1998_12
- 特許番号
- US05854245
反応ノート
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