HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → tert-butyl (3S)-3-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperidin-1-yl)methyl]piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | tert-Butyl (3R)-3-formylpiperidine-1-carboxylate | HCID 42325667 | — |
| Reactant | N-(3,4-dichlorophenyl)piperidine-4-carboxamide hydrochloride | HCID 54595048 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-butyl (3S)-3-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperidin-1-yl)methyl]piperidine-1-carboxylate | HCID 57656896 | 100% |
Reaction Steps
To a mixture of N-(3,4-dichlorophenyl)piperidine-4-carboxamide hydrochloride (1.55 g) in dichloromethane (100 mL) was added di-iso-propylethylamine (1.3 mL). The solution was stirred for 15 minutes after which tert-butyl (3R)-3-formylpiperidine-1-carboxylate (1.17 g) and sodium triacetoxyborohydride (1.59 g) was added. The reaction was stirred at room temperature overnight. The reaction mixture was partitioned between dichloromethane and water and the aqueous layer extracted with dichloromethane. The combined organic layers were washed with brine, dried over magnesium sulfate and evaporated to give the title compound as a white foam (2.34 g, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710224B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-b0520ac579164da68fab6afd729ee76d |
| Source note | uspto-grants-2014_04 |