Chlorosulfonic acid → HCID 131724895, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of 4-(3-isopropylphenoxyactamido)butyric acid 2-(3-nitrobenzenesulfonyl)ethyl ester (Intermediate 25, 4.8 g, 9.75 mmol) and 2 mL of CH2Cl2 was added drop-wise ClSO3H (3.3 mL, 5.8 g, 50 mmol) at 0° C. with vigorous stirring. The mixture was stirred at 0° C. for 40 min. and then was 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 passed through a short silica gel column to remove material that was not moving on TLC. The eluent was concentrated to give Intermediate 26 (3.3 g, 57%) as a light brown foam.

Provenance & Evidence