Methanol → 4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic acid salt

Temperatur

50 °C

Combine 1-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane (1.80 g, 4.22 mmol) and methanol (15 mL). Cool in an ice bath. Add aqueous hydriodic acid (3.8 g, 2.23 mL, 57%, 16.9 mmol) and warm to ambient temperature. After 30 minutes, add aqueous hydriodic acid (1.12 mL) and heat to 50° C. After 2 hours, cool to ambient temperature and evaporate to remove most of the methanol to give a residue. Combine the residue and methanol (10 mL). Add diethyl ether (200 mL) and stir to give a solid. Decant the solvent, add diethyl ether (200 mL) and stir, collect the solid by filtration to give, after drying, the title compound: mp; 206-208° C.

1. temperatureCool in an ice bath
2. waitAfter 2 hours
3. temperaturecool to ambient temperature
4. customevaporate
5. customto remove most of the methanol
6. customto give a residue
7. customto give a solid
8. customDecant the solvent
9. additionadd diethyl ether (200 mL)
10. customcollect the solid
11. filtrationby filtration
12. customto give
13. customafter drying

ORD-Eintrag

ord-bc415e0df799461eae7f451bbb496434

Quelldatensatz

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05932571