반응 #1914819

반응 방정식

(2,3-Dihydro-thieno[3,4-b][1,4]dioxin-2-yl)-methanol

NaH

butanesultone

→

4-(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-yl-methoxy)-butane-1-sulphonic acid sodium salt

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도to reflux for 3 h
2. 2
   기타the solvent was removed
3. 3
   workup.ADDITIONmethanol 5 was added
4. 4
   workup.STIRRINGthe mixture was stirred
5. 5
   여과filtered
6. 6
   농축the filtrate was concentrated
7. 7
   workup.ADDITIONThe remaining oil was solidified by addition of hexane and ethanol
8. 8
   workup.STIRRINGby stirring
9. 9
   여과Final filtration
10. 10
    기타drying
11. 11
    기타resulted in pure 4-(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-ylmethoxy)-butane-1-sulphonic acid sodium salt

실험 절차

(2,3-Dihydro-thieno[3,4-b][1,4]dioxin-2-yl)-methanol (6.9 g, 40 mmol) was dissolved into tetrahydrofuran (100 mL) and blanketed by nitrogen. NaH (1.76 g) was added and stirring was continued for 30 min. Then butanesultone (6.0 g) was added dropwise after which the reaction mixture was brought to reflux for 3 h. Then it was cooled to 25° C. again, the solvent was removed, methanol 5 was added, the mixture was stirred, filtered and the filtrate was concentrated. The remaining oil was solidified by addition of hexane and ethanol, followed by stirring. Final filtration and drying resulted in pure 4-(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-ylmethoxy)-butane-1-sulphonic acid sodium salt as was demonstrated by NMR and mass spectroscopy.

출처