反应 #1914819

反应方程式

(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

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度to reflux for 3 h
2. 2
   其他the solvent was removed
3. 3
   workup.ADDITIONmethanol 5 was added
4. 4
   workup.STIRRINGthe mixture was stirred
5. 5
   过滤filtered
6. 6
   浓缩the filtrate was concentrated
7. 7
   workup.ADDITIONThe remaining oil was solidified by addition of hexane and ethanol
8. 8
   workup.STIRRINGby stirring
9. 9
   过滤Final filtration
10. 10
    其他drying
11. 11
    其他resulted in pure 4-(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-ylmethoxy)-butane-1-sulphonic acid sodium salt

实验过程

(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.

来源