反応 #1914819

反応方程式

(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

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度to reflux for 3 h
2. 2
   その他the solvent was removed
3. 3
   workup.ADDITIONmethanol 5 was added
4. 4
   workup.STIRRINGthe mixture was stirred
5. 5
   ろ過filtered
6. 6
   濃縮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
   ろ過Final filtration
10. 10
    その他drying
11. 11
    その他resulted in pure 4-(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-ylmethoxy)-butane-1-sulphonic acid sodium salt

実験手順

(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.

出典