反应详情

69NLS77 (190 mg, 0.45 mmol) was N-BOC deprotected as described in the preparation of 69NLS79-II and dissolved in DMF (3 mL). Potassium carbonate (250 mg, 1.80 mmol) was added, followed by ethylbromide (50 μL, 0.45 mmol)) and the mixture stirred overnight at rt. Workup was carried out as for 69NLS79-II. The residue was purified by silica gel column chromatography, eluting with a stepwise gradient of 0-6% methanol in dichloromethane, followed by repurification of the compound by acidic ion-exchange SPE cartridge, to give 38-PH20 (77 mg, 38%) as a colourless oil. The compound was converted to its hydrochloride form by treatment with 2M HCl in diethylether as described above, giving the salt as a colorless powder.

1. customas described in the preparation of 69NLS79-II and
2. customThe residue was purified by silica gel column chromatography
3. washeluting with a stepwise gradient of 0-6% methanol in dichloromethane
4. customfollowed by repurification of the compound by acidic ion-exchange SPE cartridge
5. customto give 38-PH20 (77 mg, 38%) as a colourless oil