Pyridine → HCID 131711822, compound

Participants

Reaction Steps

8.8 g (10 mmoles) of Ddz-Cys(Trt)-Thr(But)-Ser(But)-OH are dissolved at room temperature in a mixture of 8.75 ml (0.1 mole) of trifluoroacetic acid, 1.75 ml of water and 165 ml of methylene chloride (=about 175 ml of a 5% strength solution of trifluoroacetic acid in methylene chloride, containing 1% of water). The mixture is left to stand at room temperature for 1.5 hours and is then neutralized with 8.85 ml (0.11 mole) of pyridine. The solution is concentrated and the residue is partitioned between ethyl acetate and water. The ethyl acetate phase is washed twice more with water and is dried over Na2SO4 and concentrated. The residue is dissolved in a small amount of ether and the solution is slowly added dropwise to petroleum ether.

Provenance & Evidence