反应详情

温度

0 °C

To a mixture of 3-(2-methoxyphenyl)propionic acid 2-(toluene-4-sulfonyl)ethyl ester (Intermediate 59, 5.0 g, 13.8 mmol) and 5 mL of CH2Cl2 was added dropwise chlorosulfonic acid (8.0 g, 69.0 mmol, 5.0 eq) with ice-bath cooling. The mixture was stirred at 0° C. for 30 min. The resulting thick oil was poured onto crushed ice with vigorous stirring. The mixture was extracted with EtOAc. The organic layer was dried over MgSO4, and concentrated by evaporation to give a thick oil, which was purified by column chromatography (CH2Cl2) to yield 3-(5-chlorosulfonyl-2-methoxyphenyl)propionic acid 2-(toluene-4-sulfonyl)ethyl ester (Intermediate 60, 4.7 g, 74%) as a light brown oil.

1. temperaturecooling
2. additionThe resulting thick oil was poured
3. customonto crushed ice with vigorous stirring
4. extractionThe mixture was extracted with EtOAc
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated by evaporation
7. customto give a thick oil, which
8. customwas purified by column chromatography (CH2Cl2)