反応式
[CH3:1][O:2][C:3]1[C@@H:4]([CH:11]([CH3:13])[CH3:12])[N:5]=[C:6]([O:9][CH3:10])[CH2:7][N:8]=1.C([Li])(C)(C)C.I[CH2:20][CH2:21][CH:22]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:23]([F:26])([F:25])[F:24].[Cl-].[NH4+]>O1CCCC1>[CH:11]([C@@H:4]1[C:3]([O:2][CH3:1])=[N:8][C@@H:7]([CH2:20][CH2:21][CH:22]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:23]([F:25])([F:26])[F:24])[C:6]([O:9][CH3:10])=[N:5]1)([CH3:13])[CH3:12]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of (R)-(−)-2,5-dihydro-3,6-dimethoxy-2-isopropylpyrazine (1.1 g) in tetrahydrofuran (25 ml) was cooled to −70° C., then tert.butyllithium (1.7 M in pentane, 3.88 ml) was added and the mixture was stirred for 1 hour. A solution of (3-iodo-1-trifluoromethyl-propyl)-benzene (1.98 g) in tetrahydrofuran (7 ml) was added slowly and the mixture was stirred overnight at −70° C. At room temperature saturated ammonium chloride solution was added and the mixture was extracted three times with ether. The combined organic layers were dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (SiO2, heptane/EtOAc=9:1 to yield a yellow liquid, (1.86 g, 83%).
後処理
- stirringthe mixture was stirred overnight at −70° C
- extractionthe mixture was extracted three times with ether
- dry with materialThe combined organic layers were dried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by column chromatography (SiO2, heptane/EtOAc=9:1
- customto yield a yellow liquid, (1.86 g, 83%)
出典と根拠
- ORDレコード
- ord-8b979149bfaf420d84f4f17b56e20eb0
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08242153B2
関連ノート
読み込み中…