反应详情

1-(4-Amino-quinazolin-7-ylmethyl)-4-benzyloxycarbonyl-3-(S)-(2-methylsulfanyl-ethyl)-piperazin-2-one (100 mg, 0.215 mmol) is dissolved in 5 ml of 30% hydrogen bromide in acetic acid. The mixture is stirred for 1 hour, diluted with ethyle ether. The ether is decanted and the resulting solid is washed thoroughly with ethyle ether. The resulting crude product is purified by column chromatography eluting with a 4/2/1 mixture of CH2Cl2/MeOH/NH4OH (30% in H2O). with a gradient of 5% MeOH:CH2Cl2 to 10% MeOH:CH2Cl2. The resulting product is purified by another column chromatography eluting with a gradient of 20% MeOH:CH2Cl2 to 50% MeOH:CH2Cl2. The title bound (30 mg, 42% yield) is obtained as an off-white solid.

1. customThe ether is decanted
2. washthe resulting solid is washed thoroughly with ethyle ether
3. customThe resulting crude product is purified by column chromatography
4. washeluting with a 4/2/1 mixture of CH2Cl2/MeOH/NH4OH (30% in H2O)
5. customThe resulting product is purified by another column chromatography
6. washeluting with a gradient of 20% MeOH
7. customis obtained as an off-white solid