反応 #345968

反応方程式

2-mercaptoethanol

methanol

sodium mercaptide

2-mercaptoethanol

1,3-dichloropropane

sodium methoxide

→

crude product

収率 95.0%

1,3-Bis(2-hydroxyethylthio)propane

収率 95.0%

反応条件

後処理

1. 1
   温度the mixture was refluxed for 1 hour
2. 2
   ろ過filtered
3. 3
   その他The methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol
4. 4
   workup.DISTILLATIONwere distilled off at high vacuum at room temperature
5. 5
   抽出The yellow, oily residue was extracted with acetone
6. 6
   ろ過the solution filtered
7. 7
   その他the acetone evaporated

実験手順

The sodium mercaptide of 2-mercaptoethanol was made by reacting 1 mole each of sodium methoxide and 2-mercaptoethanol in dry methanol under a nitrogen atmosphere. To this solution, 0.5 mole of 1,3-dichloropropane was added and the mixture was refluxed for 1 hour and filtered. The methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol were distilled off at high vacuum at room temperature. The yellow, oily residue was extracted with acetone, the solution filtered, and the acetone evaporated to give a 95 percent yield of the crude product.

出典