HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → 2-(2-Amino-thiazol-4-yl)-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone trihydrobromide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | (4-{2-[4-(1-Methyl-piperidin-4-yl)-piperazin-1-yl]-2-oxo-ethyl}-thiazol-2-yl)-carbamic acid tert-butyl ester | HCID 59698869 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 2-(2-Amino-thiazol-4-yl)-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone trihydrobromide | HCID 86606002 | — |
Reaction Steps
47.2 To a stirred suspension of 3.9 g (4-{2-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-2-oxo-ethyl}-thiazol-2-yl)-carbamic acid tert-butyl ester was added 40 ml of 33% HBr in acetic acid. The reaction mixture was stirred at r.t. for 4 h. The mixture was left overnight in the fridge. Then it was concentrated to leave an off-white solid which was suspended in 50 ml Et2O, triturated and stirred at r.t. for 3 h. The product was collected by filtration, washed with Et2O and dried to give 5.6 g 2-(2-amino-thiazol-4-yl)-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-ethanone trihydrobromide. Off-white solid. MS 324.4 ([M+H]+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361672B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-30c1679e95d24b9897ef17378014617c |
| Source note | uspto-grants-2008_04 |