反应 #1597030

反应方程式

MsCl

MsCl

(2,3-dihydro-4-oxa1-thia-6-aza-naphthalen-7-yl)-methanol

NaHCO3

→

compound

收率 100.5%

Methanesulfonic acid 2,3-dihydro-4-oxa-1-thia-6-aza-naphthalen-7-ylmethyl ester

收率 100.5%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   其他The two layers were decanted
2. 2
   干燥layer was dried over Na2SO4
3. 3
   过滤filtered
4. 4
   浓缩concentrated to dryness
5. 5
   其他The residue was purified by CC (DCM-MeOH 97-3)

实验过程

To a suspension of (2,3-dihydro-4-oxa1-thia-6-aza-naphthalen-7-yl)-methanol (0.150 g, 0.8 mmol; prepared as described in WO 2004/058144) in DCM (4 mL), cooled to 0° C., were added TEA (0.228 mL, 1.6 mmol, 2 eq.) and MsCl (0.076 mL, 0.98 mmol, 1.2 eq.). The reaction was stirred at the same temperature. MsCl (0.013 mL, 0.16 mmol) was added after 30 min. A sat. NaHCO3 solution (25 mL) and DCM (20 mL) were added. The two layers were decanted and the org. layer was dried over Na2SO4, filtered and concentrated to dryness. The residue was purified by CC (DCM-MeOH 97-3) to afford the tittle compound as a yellowish oil (0.210 g, 98% yield).

来源