Methanol → HCID 86756616, compound

Participants

Reaction Steps

MeOH (5 mL) was cooled with an ice-acetone bath, and thionyl chloride (60 μL) was added. This solution was stirred for 1 min, and then the amino acid from Example 7 (163 mg, 0.70 mmol) was added all at once. After removing the cooling bath, the reaction was stirred while warming to ambient temperature over 1 hr, and then heated to 40° C. for another 1.5 hr. When the reaction mixture was concentrated to dryness, HPLC analysis of the residue indicated that the reaction was incomplete, so the above reaction sequence was repeated, this time heating the reaction for 0.5 hr at the end. The reaction mixture was concentrated to dryness, giving the product as a light yellow solid (168 mg, 97%).

Provenance & Evidence