Ammonia → HCID 131714506, compound

Participants

Reaction Steps

5.00 g (4.28 mmol) of BOC-Val-Pro-Pro-Leu-Gly-Trp-Met-OMe (XI) prepared in Example 1, Step 11, were dissolved in a solution of 100 ml of methanol and 2 ml of ethylene glycol, and saturated at 0° C. with ammonia. The reaction mixture was kept in the refrigerator for 3 days, and then the excess of ammonia and the solvent were removed in vacuo. The crude product was partially purified by column chromatography on silica gel (Merck) 0.040-0.063 mm eluting with AcOEt:MeOH=87:13 and used as such in the next Step (2.58 g of compound XV were obtained from iPrOH/iPr2O): RfC 0.31.

Provenance & Evidence