Chloroform → 1,4-di(3,3,4,4,5,5,6,6,6-nonafluorohexyl) 2-(N,N-dimethylaminoethanethionyl)maleate
反応式
[C:1]([O:23][CH2:24][CH2:25][C:26]([F:38])([F:37])[C:27]([F:36])([F:35])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30])(=[O:22])/[CH:2]=[CH:3]\[C:4]([O:6][CH2:7][CH2:8][C:9]([F:21])([F:20])[C:10]([F:19])([F:18])[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])=[O:5].Cl.CN([CH:43]([SH:45])C)C.C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)Cl.[CH3:56][N:57]([CH3:60])[CH:58]=O>>[CH3:56][N:57]([CH2:58][C:43](/[C:2](=[CH:3]/[C:4]([O:6][CH2:7][CH2:8][C:9]([F:21])([F:20])[C:10]([F:18])([F:19])[C:11]([F:17])([F:16])[C:12]([F:15])([F:14])[F:13])=[O:5])/[C:1]([O:23][CH2:24][CH2:25][C:26]([F:37])([F:38])[C:27]([F:35])([F:36])[C:28]([F:33])([F:34])[C:29]([F:32])([F:31])[F:30])=[O:22])=[S:45])[CH3:60]参加物
6
反応物 5
生成物 1
反応条件
- 温度
- 60 °C
実験手順
In an amount of 25.1 g (41 mmol) of 1,4-di(3,3,4,4,5,5,6,6,6-nonafluorohexyl) maleate, 6.4 g (45 mmol) of N,N-di-methylaminoethanethiol hydrochloride and 5.7 g (41 mmol) of potassium carbonate were dissolved in 60 mL of N,N-dimethylformamide and stirred at 60° C. for 4 hours. Then, the reaction mixture was added with 500 mL of chloroform and the organic phase was washed with a saturated aqueous sodium hydrogencarbonate solution. Subsequently, the organic layer was collected, and the organic solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:2 to 0:10 (volume ratio)) to obtain 15.8 g (yield: 54%) of the target compound.
後処理
- washthe organic phase was washed with a saturated aqueous sodium hydrogencarbonate solution
- customSubsequently, the organic layer was collected
- customthe organic solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:2 to 0:10 (volume ratio))
出典と根拠
- ORDレコード
- ord-71d231a652584729a570b5ad7e042ac1
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06933101B2
反応ノート
読み込み中…