Dimethyl Sulfide → HCID 131716950, compound

Participants

Reaction Steps

The dried resin peptide (1 g) was premixed with dimethylsulfide, p-thiocresol, and p-cresol; liquid HF at -78° C. was then added to give approximately a final volume of 10 mL (65:2.5:7.5:25 by volume). The mixture was equilibrated to 0° C. by stirring in an ice bath. After 2 hr, the HF and dimethyl sulfide were removed in vacuo. The high HF treatment was initiated by recharging the reaction vessel at -78° C. with about 14 mL of fresh HF to give a total volume of 15 mL HF-p-cresol-p-thiocresol. The reaction was carried out at 0° for 1 hr. After evaporation of HF at 0° C. and washing with cold ether, the crude reaction mixture was extracted with 10% aqueous acetic acid. The mixture was then lyophilized to dryness.

Provenance & Evidence