Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Sitagliptin | HCID 4369359 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 44131507 | HCID 44131507 | — |
Reaction Steps
Sitagliptin (5 g) and isopropanol (75 mL) are charged into a round-bottom flask and the mixture is heated to about 80° C. for about 30 minutes to obtain a clear dissolution. Hydrobromic acid (2.1 g) is added and the reaction mixture is refluxed for about 1.5 hours. The reaction mixture is cooled to about 30° C. and stirred for about 22 hours. The separated solid is filtered, washed with isopropanol (5 mL), and dried under reduced pressure at about 35° C. for about 1.25 hours to afford the title compound. (Yield: 4.0 g; MC: 2.40% w/w; HPLC purity: 99.70%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08309724B2 |
|---|
| Source dataset | uspto-grants-2012_11 |
|---|
| ORD ID | ord-897d5f2cee614702a0198a0787515825 |
|---|
| Source note | uspto-grants-2012_11 |
|---|