反应详情

N-Benzyl-N′,N′-dimethyl-N-[3-(1-trityl-1H-benzotriazol-5-yl)-benzyl]-propane-1,3-diamine (60 mg, 0.093 mmol) was dissolved in a mixture of 5 mL of ethanol, 5 mL of dioxane and 8 mL of 2M aqueous hydrochloric acid solution, and the resulting mixture was stirred at room temperature for 6 h. The volatiles were removed in vacuo and the residue partitioned between diethyl ether and 1M HCl solution. The aqueous phase was washed with diethyl ether and the combined organic phases were concentrated in vacuo to obtain the crude product, which was dissolved in small amount of 1M HCl solution and freeze dried. Purification by HPLC (elution with 30% acetonitrile/70% water (containing 0.1% trifluoroacetic acid)) afforded 30 mg of the title compound. LC/MS (short method): Retention time 1.19 min; (M+H)=400.

1. customThe volatiles were removed in vacuo
2. customthe residue partitioned between diethyl ether and 1M HCl solution
3. washThe aqueous phase was washed with diethyl ether
4. concentrationthe combined organic phases were concentrated in vacuo
5. customto obtain the crude product, which
6. customdried
7. customPurification
8. washby HPLC (elution with 30% acetonitrile/70% water (containing 0.1% trifluoroacetic acid))