HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → tert-butyl (2S)-2-methyl-4-[2-methyl-4-(methylamino)benzyl]piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | tert-Butyl (2S)-2-methylpiperazine-1-carboxylate | HCID 10081508 | — |
| Reactant | 2-Methyl-4-(methylamino)benzaldehyde | HCID 45083649 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | tert-butyl (2S)-2-methyl-4-[2-methyl-4-(methylamino)benzyl]piperazine-1-carboxylate | HCID 59262129 | 37% |
Reaction Steps
To a mixture of 2-methyl-4-(methylamino)benzaldehyde (D93) (0.397 g) and 1,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate (0.533 g, 2.66 mmol) in 1,2-DCE (35 mL) was added sodium tri(acetoxy)borohydride (0.847 g, 4.00 mmol) and the reaction stirred at room temperature overnight. Saturated aqueous NaHCO3 (30 mL) was added and the mixture was stirred for 4 h. The reaction mixture was extracted with DCM and the organics were dried and concentrated to give the crude product which was purified by column chromatography. Elution with ether/petroleum ether gave the title compound as a colourless oil (0.328 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853218B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-14d63a0ce4454544a58db7da5952d504 |
| Source note | uspto-grants-2014_10 |