Tetrahydrofuran → HCID 17878496, compound

Participants

Reaction Steps

Following Synthesis Method (A), into 200 ml of anhydrous tetrahydrofuran (hereinafter referred to as THF) was dissolved 4.90 g (22.5 mmol) of 4-chlorobenzenesulfonylisocyanate, then 3.51 g (20.5 mmol) of 2-amino-4-chlorobenzoic acid was added and the mixture was stirred at room temperature for two hours. The reaction solution was cooled by ice water, then 3.98 g (24.55 mmol) of CDI was added and the mixture was stirred under ice cooling for 30 minutes. An excess amount of water was poured into the reaction solution, then the precipitated crystal was obtained by filtration and the obtained crystal was washed by water, then was washed by ethyl acetate to obtain 5.03 g of the above-identified compound (yield 66.5%). Properties: colorless crystal, Melting point: 286°-287° C., PMR (δppm, DMSO-d6): 7.12 (1H,s), 7.23 (1H,d), 7.26 (2H,d), 7.86 (1H,d), 8.17 (2H,d), 11.71 (1H,br).

Provenance & Evidence