反应详情

A mixture of 4.6 g of benzilic acid, 3.2 g of 1,1'-carbonyldiimidazole, and 150 ml of DMF were mixed and stirred for 1 hour. A solution of 5.0 g of 4-amino-α-hexyl-1H-imidazole-1-acetic acid ethyl ester in DMF was added and the mixture stirred at room temperature over-night. The reaction mixture was concentrated in vacuo, ethyl acetate was added, and the organic solution was washed sequentially with water, a 10% sodium hydroxide solution, and water. The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by HPLC eluting with 30% ethyl acetate in toluene. The appropriate fractions were combined and concentrated in vacuo to provide 1.4 g of the desired titled product.

1. additionwere mixed
2. stirringthe mixture stirred at room temperature over-night
3. concentrationThe reaction mixture was concentrated in vacuo, ethyl acetate
4. additionwas added
5. washthe organic solution was washed sequentially with water
6. dry with materialThe organic layer was dried over sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by HPLC
9. washeluting with 30% ethyl acetate in toluene
10. concentrationconcentrated in vacuo