反応式
[CH2:1]([N:8]([CH3:12])[CH2:9][CH2:10][OH:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.CS(C)=O.N1C=CC=CC=1.S(=O)(=O)=O>C(Cl)Cl>[CH2:1]([N:8]([CH2:9][CH:10]=[O:11])[CH3:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
6
反応条件
- 温度
- -10 °C
実験手順
To a 3-necked 2-L flask was added N-benzyl-N-methylethanolamine (30.5 g, 0.182 mol), DCM (0.5 L), DIPEA (95 mL, 0.546 mol) and DMSO (41 mL, 0.728 mol). Using an ice bath, the mixture was cooled to about −10° C. and sulfur trioxide pyridine-complex (87 g, 0.546 mol) was added in 4 portions over 5 minutes intervals. The reaction was stirred at −10° C. for 2 hours. Before removing the ice-bath, the reaction was quenched by adding water (0.5 L). The aqueous layer was separated and the organic layer was washed with water (0.5 L) and brine (0.5 L) and then dried over magnesium sulfate and filtered to provide the title compound which was used without further purification.
後処理
- customBefore removing the ice-bath
- customthe reaction was quenched
- additionby adding water (0.5 L)
- customThe aqueous layer was separated
- washthe organic layer was washed with water (0.5 L) and brine (0.5 L)
- dry with materialdried over magnesium sulfate
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-212e87e68da146c2aaa0e1b619618666
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08067439B2
関連ノート
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