反应详情

温度

50 °C

Stir a solution of 4-[1-(2,2,2-trifluoro-ethyl)-1H-benzoimidazol-2-yl]-[1,4]diazepane-1-carboxylic acid tert-butyl ester (0.43 g, 1.07 mmol), methanol (10 mL) and 57% hydroiodic acid overnight at room temperature, and then heat for two hours at 50° C. Cool, add 57% hydroiodic acid (1 mL) and heat for two hours. Concentrate in vacuo to remove the solvents, dilute the residue with methanol (150 mL), concentrate in vacuo, and triturate the residual oil with ether (300 mL) to afford a tan solid. Stir the mixture for one hour, collect the solid by vacuum filtration under nitrogen, and dry in vacuo (0.2 Torr) at 82° C. to afford 0.54 g of 2-[1,4]diazepan-1-yl-1-(2,2,2-trifluoro-ethyl)-1H-benzoimidazole dihydroiodide, m.p. >225° C. Elemental Analysis: Calculated for C14H19F3N4.2HI: 30.35%C, 3.46%H, 10.11%N; Found 30.46%C, 3.33%H, 9.79%N.

1. temperatureCool
2. temperatureheat for two hours
3. concentrationConcentrate in vacuo
4. customto remove the solvents
5. additiondilute the residue with methanol (150 mL)
6. concentrationconcentrate in vacuo
7. customtriturate the residual oil with ether (300 mL)
8. customto afford a tan solid
9. customcollect the solid
10. filtrationby vacuum filtration under nitrogen
11. customdry in vacuo (0.2 Torr) at 82° C.