반응 #1244243

반응 방정식

HOCH2CH2ONa

methanol

FSO2CH2CH2Cl

THF

→

crude product

FSO2CH2CH2OCH2CH2OH

용매

dichloromethane

water

반응 조건

후처리

1. 1
   온도under cooling with ice bath
2. 2
   온도while maintaining the internal temperature
3. 3
   기타to be at most 10° C
4. 4
   workup.ADDITIONAfter completion of the dropwise addition, it
5. 5
   workup.STIRRINGwas stirred at room temperature for 2 hours
6. 6
   workup.ADDITIONwas added
7. 7
   기타The obtained crude liquid
8. 8
   기타was subjected to liquid separation
9. 9
   추출the obtained aqueous layer was extracted with dichloromethane (124 g)
10. 10
    추출The separated aqueous layer was further extracted with dichloromethane (126 g)
11. 11
    건조It was dried over magnesium sulfate
12. 12
    여과after filtration
13. 13
    workup.DISTILLATIONthe solvent was distilled off

실험 절차

Into a round flask, HO(CH2)2OH (140.9 g) and a methanol solution of sodium methylate (28 wt %, 96.4 g) were charged and stirred, and heated under reduced pressure to distill off methanol thereby to obtain a solution of HOCH2CH2ONa. It was confirmed by GC that no methanol remained in the reaction solution. Into a four necked flask, FSO2CH2CH2Cl (50 g) and THF (100 mL) were charged and stirred under cooling with ice bath, and the previously obtained solution of HOCH2CH2ONa was dropwise added thereto over a period of 2.5 hours, while maintaining the internal temperature to be at most 10° C. After completion of the dropwise addition, it was stirred at room temperature for 2 hours and then added to water (400 mL), and dichloromethane (183 g) was added. The obtained crude liquid was subjected to liquid separation, and the obtained aqueous layer was extracted with dichloromethane (124 g). The separated aqueous layer was further extracted with dichloromethane (126 g), and the organic layers were put together. It was dried over magnesium sulfate, and after filtration, the solvent was distilled off to obtain a crude product (47.1 g). The obtained crude liquid was used for the next step without carrying out purification.

출처