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(dodecylthio)acetic acid synthesis

5synthesis methods
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Yield:13753-71-4 92%

Reaction Conditions:

Stage #1: 1-dodecylthiolwith sodium hydroxide in ethanol at 20; for 0.5 h;
Stage #2: chloroacetic acidwith sodium hydrogencarbonate in ethanol;water; for 2 h;

Steps:

1.1 Example 1(Preparation of (2- (dodecylsulfinyl) -N - ((tetrahydrofuran-2-yl) methyl) acetamide (1)

In a 500 ml round bottom flask, 20.2 g of dodecyl alcohol, 300 ml of anhydrous ethanol, 4 g of sodium hydroxide,Stirring at room temperature for 0.5 hours to completely dissolve the sodium hydroxide;To a 100 ml beaker was added 9.5 g of chloroacetic acid, 20 ml of water,5 g of sodium bicarbonate was added 3 times with stirring, stirred until the solid was completely dissolved;The dropping solution was slowly added dropwise (dripping at a rate of 1 drop / sec) into the flask under mechanical agitation. After completion of the dropwise addition, stirring was continued for 2 hours,The residue was added to a 500 ml flask,Add 200 ml of 1 mol / L dilute hydrochloric acid, 100 ml of ethyl acetate, shake well,After stratification, take the upper organic phase, remove the ethyl acetate by steaming,2-dodecylthioAcetic acid 23.92 g, yield 92%;

References:

CN106478557,2017,A Location in patent:Paragraph 0045; 0046; 0047