1,1-Dichloroethane → HCID 15622949、化合物
反応式
[CH3:1][CH:2]([CH3:14])[CH2:3][O:4][CH2:5][CH:6]([OH:13])[CH2:7][N:8]1[CH2:12][CH2:11][CH2:10][CH2:9]1.ClC(Cl)C.S(Cl)(Cl)=O.[OH-].[Na+]>>[CH3:14][CH:2]([CH3:1])[CH2:3][O:4][CH2:5][CH:6]([OH:13])[CH2:7][N:8]([CH2:9][CH3:10])[CH2:12][CH3:11]参加物
5
実験手順
10 g. 3-(2-Methylpropoxy)-1-pyrrolidinopropan-2-ol are dissolved in 100 ml. dichloroethane. A solution of 7.1 g. thionyl chloride in 20 ml. dichloroethane is added dropwise thereto, while stirring, and the reaction mixture subsequently heated for 2 hours to 70° C. The reaction mixture is cooled, poured on to ice water and subsequently rendered alkaline by the addition of a concentrated aqueous solution of sodium hydroxide. The organic phase is separated off and the aqueous phase again extracted with methylene chloride. The organic phases are combined, dried over anhydrous sodium sulphate and evaporated. The residue is purified by chromatography on a silica gel column (elution agent: methylene chloride/5% methanol). There are obtained 9 g. of the title compound in the form of an oily product.