反应详情

2-(1,4-Diazepan-1-yl)ethanol (311 mg) was added to a suspension of the product of Example 75 step i) (301 mg) in dichloromethane (5 mL). The reaction was stirred at room temperature for 1 hour before the addition of sodium triacetoxyborohydride (457 mg). The reaction was then stirred at room temperature for 1 hour. The reaction mixture was treated with methanol (2 mL) and then concentrated to dryness. The resulting material was purified by HPLC then by SCX ion exchange chromatography (eluting with methanol followed by 1.5M methanolic ammonia). The fractions containing product were concentrated to dryness and the residue triturated with acetonitrile to afford the title compound as a solid (300 mg).

1. concentrationconcentrated to dryness
2. customThe resulting material was purified by HPLC
3. washby SCX ion exchange chromatography (eluting with methanol followed by 1.5M methanolic ammonia)
4. additionThe fractions containing product
5. concentrationwere concentrated to dryness
6. customthe residue triturated with acetonitrile