Hydrochloric Acid → Hydantoin, 5,5-dimethyl-3-(p-fluorophenyl)-
反応式
CO[C:3](=[O:18])[C:4]([CH3:17])([CH3:16])[NH:5][C:6](=[O:15])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1.Cl>CC(C)=O>[F:14][C:11]1[CH:10]=[CH:9][C:8]([N:7]2[C:3](=[O:18])[C:4]([CH3:16])([CH3:17])[NH:5][C:6]2=[O:15])=[CH:13][CH:12]=1参加物
4
実験手順
A solution of 17.2 g (67.5 mmol) of N-[(4-fluorophenyl)-carbamoyl]-2-methylalanine methyl ester in 150 ml of 6-N aqueous hydrochloric acid and 50 ml of acetone was warmed on a steam bath for 2 hours. The mixture was then concentrated. The product, which had precipitated was dried at 40°/15 Torr and then recrystallized from toluene. The recrystallized product was dried at 50° C. for 20 hours, under greatly reduced pressure, to yield 3-(4-fluorophenyl)-5,5-dimethylhydantoin, m.p. 166°-167° C.
後処理
- concentrationThe mixture was then concentrated
- customThe product, which had precipitated
- customwas dried at 40°/15 Torr
- customrecrystallized from toluene
- customThe recrystallized product was dried at 50° C. for 20 hours, under greatly reduced pressure
出典と根拠
- ORDレコード
- ord-b60f5cc87b134a799e38f69e1866db4b
- 出典データセット
- uspto-grants-1980_11
- 特許番号
- US04234736
反応ノート
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