反应详情

温度

0 °C

To a solution of [2-(2-benzenesulfonyl-ethoxycarbonylmethoxy)phenoxy]acetic acid 2-benzenesulfonyl-ethyl ester (Intermediate 28, 7.4 g, 13.2 mmol) in 10 mL of CH2Cl2 was added drop-wise ClSO3H (5.0 mL, 8.8 g, 75.8 mmol, 5.7 eq) at 0° C. with vigorous stirring. The mixture was stirred at 0° C. for 1.5 h. and then poured onto crushed ice with vigorous stirring, resulting in a thick mass. This was extracted with CH2Cl2. The organic layers were dried and concentrated under reduced pressure. The residual oil was dried under vacuum overnight to give Intermediate 29 (8.0 g, 92%) as an off-white foam.

1. additionpoured
2. customonto crushed ice with vigorous stirring
3. customresulting in a thick mass
4. extractionThis was extracted with CH2Cl2
5. customThe organic layers were dried
6. concentrationconcentrated under reduced pressure
7. customThe residual oil was dried under vacuum overnight