تفاعل #524798

معادلة التفاعل

sodium bicarbonate

4-mercapto-2-butanol

n-decanal

p-toluene sulfonic acid

→

6-methyl-2-nonyl-1,3-oxathiane

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONBoiling chips are added to the flask
2. 2
   workup.DISTILLATIONA Dean-Starke distilling receiver
3. 3
   درجة الحرارةThe flask is then heated slowly
4. 4
   درجة الحرارةuntil reflux
5. 5
   درجة الحرارةthe temperature is increased for a more vigorous reflux
6. 6
   أخرىThe reflux lasts for a period of 2 hours before water of reaction ceases
7. 7
   أخرىto be formed
8. 8
   درجة الحرارةThe reaction mass is then cooled
9. 9
   ترشيحThe reaction mass is filtered
10. 10
    ترشيحthrough fluted filter paper
11. 11
    أخرىthe dichloromethane solvent is removed by means of rotary evaporation
12. 12
    أخرى11.8 grams of crude product are recovered after the rotary evaporation operation
13. 13
    workup.DISTILLATIONThe crude product is then distilled by means of vacuum distillation
14. 14
    أخرىyielding the following 4 fractions

الإجراء التجريبي

75 ml of dichloromethane is placed in a 100 ml round-bottom flask. To the dichloromethane is added 5.3 grams (0.05 moles) of 4-mercapto-2-butanol. 8.58 grams (0.055 moles) n-decanal is then added followed by 0.1 grams of p-toluene sulfonic acid. Boiling chips are added to the flask. A Dean-Starke distilling receiver is placed on the flask, and a reflux condenser is placed on the receiver. The flask is then heated slowly until reflux occurs, and then the temperature is increased for a more vigorous reflux. The reflux lasts for a period of 2 hours before water of reaction ceases to be formed. The reaction mass is then cooled and neutralized with 10% aqueous sodium bicarbonate to a pH of 8. The reaction mass is filtered through fluted filter paper, and the dichloromethane solvent is removed by means of rotary evaporation. 11.8 grams of crude product are recovered after the rotary evaporation operation. The crude product is then distilled by means of vacuum distillation yielding the following 4 fractions:

المصدر