Water → Mofegiline
反応式
C(Cl)(=O)C(Cl)=O.C[N:8]([CH3:11])C=O.[F:12]/[CH:13]=[C:14](\[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1)/CO.O>C1(C)C=CC=CC=1>[NH2:8][CH2:11]/[C:14](=[CH:13]/[F:12])/[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1参加物
6
反応条件
- 温度
- -5 °C
実験手順
Combine oxalyl chloride (25.2 g, 0.198 mol) and toluene (200 mL). Cool to -5° C. Add N,N-dimethylformamide (15.0 g, 0.21 mol) as a solution in toluene (20 mL). Warm to 25° C. After 30 minutes, add a solution of (E)-2-(fluoromethylene)-4-(p-fluorophenyl)butan-1-ol (24.7 g, 30% by weight in toluene, 0.124 mol). After 18 hours, add water (500 mL) and stir for 30 minutes. Separate the organic layer, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.
後処理
- temperatureWarm to 25° C
- waitAfter 18 hours
- customSeparate the organic layer
- dry with materialdry over Na2SO4
- filtrationfilter
- customevaporate in vacuo
出典と根拠
- ORDレコード
- ord-8f3903f462b1476ba63f6d8904e638fa
- 出典データセット
- uspto-grants-1997_10
- 特許番号
- US05679854
反応ノート
読み込み中…