反応式
C(N(CC)CC)C.[OH:8][C@H:9]([CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11].[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl>[CH3:23][S:24]([O:8][C@H:9]([CH2:15][CH2:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11])(=[O:26])=[O:25]参加物
実験手順
Triethylamine (583 mg) was added dropwise to a stirred mixture of ethyl (R)-2-hydroxy-4-phenylbutyrate (1.0 g) and methanesulfonyl chloride (660 mg) in dichloromethane (10 ml) at ice-bath temperature. After 40 minutes, the reaction mixture was partitioned between dichloromethane and water. The organic layer was washed with brine, dried over magnesium sulfate, and concentrated in vacuo to give ethyl (R)-2-methylsulfonyloxy-4-phenylbutyrate (1.37 g) as an oil. This material was used immediately without further purification. NaH (60% in mineral oil, 192 mg) was added to a solution of 4-imidazolecarboxamide (534 mg) in DMF (8 ml) at room temperature. The reaction mixture was stirred for 30 minutes. The methanesulfonate prepared above was added and the resulting mixture was stirred for 3 hours at 60° C.
後処理
- customthe reaction mixture was partitioned between dichloromethane and water
- washThe organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-8533e20906c04d8ca834359ae849788c
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06359145B1
関連ノート
読み込み中…