Trifluoroacetic acid → HCID 178458929、化合物
反応式
[Br:1][C:2]1[N:6]=[C:5]([O:7][CH2:8][CH2:9][CH3:10])[N:4](COCC[Si](C)(C)C)[C:3]=1[CH:19]=[O:20].C(O)(C(F)(F)F)=O>>[Br:1][C:2]1[N:6]=[C:5]([O:7][CH2:8][CH2:9][CH3:10])[NH:4][C:3]=1[CH:19]=[O:20]参加物
3
反応条件
- 温度
- 0 °C
実験手順
5-Bromo-2-propoxy-3-(2-trimethylsilanylethoxymethyl)-3H-imidazole-4-carbaldehyde (43.6 g, 120 mmol) was cooled at 0° C. in ice. TFA (200 mL, 2 mol) was added and the mixture was stirred at 0° C. for 15 minutes, then warmed to room temperature. After 20 minutes, the mixture was concentrated under reduced pressure and redissolved in EtOAc (300 mL). The organic was washed with saturated bicarbonate (200 mL), saturated aqueous NaCl, dried over MgSO4 and concentrated under reduced pressure to produce the title compound (28.6 g) as a yellow solid, which was used without further purification.
後処理
- temperaturewarmed to room temperature
- waitAfter 20 minutes
- concentrationthe mixture was concentrated under reduced pressure
- dissolutionredissolved in EtOAc (300 mL)
- washThe organic was washed with saturated bicarbonate (200 mL), saturated aqueous NaCl
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-ce4826f872e1425eb0fe26dcb6a230fd
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08232306B2
反応ノート
読み込み中…