HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → 1,1-Dimethylethyl (2S)-4-[(6-amino-4-methyl-3-pyridinyl)methyl]-2-methyl-1-piperazinecarboxylate
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 | 6-Amino-4-methylnicotinaldehyde | HCID 55284670 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | 1,1-Dimethylethyl (2S)-4-[(6-amino-4-methyl-3-pyridinyl)methyl]-2-methyl-1-piperazinecarboxylate | HCID 59262175 | 53.6% |
Reaction Steps
A mixture of 6-amino-4-methyl-3-pyridinecarbaldehyde (D99) (0.053 g, 0.39 mmol), 1,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate (0.117 g, 0.58 mmol) and sodium tri(acetoxy)borohydride (0.206 g, 0.97 mmol) in 1,2-DCE (10 mL) was sonicated to aid dissolution of the starting material then stirred at room temperature overnight. Saturated aqueous NaHCO3 (30 mL) was added and the mixture was stirred for 24 h. The reaction mixture was extracted with DCM (3×10 mL) and the organics were dried and concentrated to give the crude title compound as an oil (0.067 g) which was used in the next step without further purification. MS (ES): MH+ 321.3, MNa+ 343.3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07700599B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-dede3eaa4a914d8abb62d2be7be2d646 |
| Source note | uspto-grants-2010_04 |