反応式
Cl[C:2]([C@H:4]1[C@@H:6](/[CH:7]=[C:8](\[Cl:13])/[C:9]([F:12])([F:11])[F:10])[C:5]1([CH3:15])[CH3:14])=[O:3].[Cl:16][C:17]1[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[C:18]=1[CH2:19][OH:20].N1C=CC=CC=1.C1(C)C=CC=CC=1>C(OCC)C>[Cl:13]/[C:8](/[C:9]([F:12])([F:11])[F:10])=[CH:7]\[C@@H:6]1[C@H:4]([C:2]([O:20][CH2:19][C:18]2[C:21]([F:25])=[CH:22][CH:23]=[CH:24][C:17]=2[Cl:16])=[O:3])[C:5]1([CH3:15])[CH3:14]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 25 °C
実験手順
A mixture of (±)-cis-1-chlorocarbonyl-3-(Z-2-chloro-3,3,3-trifluoroprop-1-en-1-yl)-2,2-dimethylcyclopropane (0.82 g), 2-chloro-6-fluorobenzyl alcohol (1.0 g), pyridine (0.275 g) and dry toluene (50 ml) was stirred at the ambient temperature (ca. 25° C.) for a period of 6 hours and then kept for a further period of 72 hours without stirring. The mixture was diluted with diethyl ether (350 ml) and the resultant mixture washed with water, with dilute aqueous sodium carbonate solution, and then dried over anhydrous magnesium sulphate. The solvents were evaporated and the residual oil purified by preparative thick layer chromatography using silica gel plates and diethyl ether as eluent. The oil which was obtained was then distilled to yield 2-chloro-6-fluorobenzyl(±)-cis-3-(Z-2-chloro-3,3,3-trifluoroprop-1-en-1-yl)-2,2-dimethylcyclopropane carboxylate (0.67 g) b.p. 150°/0.05 mm Hg.
後処理
- waitkept for a further period of 72 hours
- stirringwithout stirring
- washthe resultant mixture washed with water, with dilute aqueous sodium carbonate solution
- dry with materialdried over anhydrous magnesium sulphate
- customThe solvents were evaporated
- customthe residual oil purified by preparative thick layer chromatography
- customThe oil which was obtained
- distillationwas then distilled
出典と根拠
- ORDレコード
- ord-bf7e88d1d9194f63a1b95ac782fe02b5
- 出典データセット
- uspto-grants-1986_01
- 特許番号
- US04567199
関連ノート
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