反応式
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH2:10]([O:13][C:14]1[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=1)[CH:11]=[CH2:12].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.C(OCC)C>[CH2:10]([O:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)=[CH:16][CH:15]=1)[CH:11]=[CH2:12]参加物
6
反応条件
- 温度
- 100 °C
実験手順
4-Fluorobenzaldehyde (3.8 mL, 35.1 mmoles) was added to a solution of the product from Example 60A (4.39 g, 29.3 mmoles) and K2CO3 (8.90 g, 64.4 mmoles) in DMF (29.3 mL). The resulting mixture was heated to 100° C. for 2.5 days and then cooled to room temperature. The crude products were diluted with diethyl ether, extracted with sat. NH4Cl, extracted with H2O (2×), washed with brine, dried (Na2SO4), and concentrated under reduced pressure. The residue was purified by flash chromatography on a prepacked Biotage column (hexane→9:1 hexane:ethyl acetate) on silica gel to provide the title compound (3.50 g, 81%) as a clear colorless oil.
後処理
- temperaturecooled to room temperature
- extractionextracted with sat. NH4Cl
- extractionextracted with H2O (2×)
- washwashed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customThe residue was purified by flash chromatography on a prepacked Biotage column (hexane→9:1 hexane:ethyl acetate) on silica gel
出典と根拠
- ORDレコード
- ord-6ec84693bfce4f2ba7bac6e36062ed87
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06583180B2
関連ノート
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