HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Benzyl 4-amino-4-cyanopiperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Benzyl 4-oxopiperidine-1-carboxylate | HCID 643496 | — |
| Solvent | Ammonia | HCID 222 | — |
| Product | Benzyl 4-amino-4-cyanopiperidine-1-carboxylate | HCID 53217057 | 62.8% |
Reaction Steps
A solution of sodium cyanide (1052 mg, 21.5 mmol), ammonium chloride (1265 mg, 23.65 mmol), and benzyl 4-oxo-1-piperidine-carboxylate (5.0 gm, 21.5 mmol), was prepared in 5 M ammonia in methanol (8.6 mL, 43 mmol). The solution was brought to reflux for 4 h and then allowed to cool to room temperature. The solution was then filtered and washed with methanol (100 mL) and the filtrate was concentrated in vacuo. The resulting oil was taken up in MTBE (250 mL) and filtered again. The filter cake was washed with MTBE (100 mL) and the filtrate was concentrated in vacuo to yield 4-amino-4-cyano-piperidine-1-carboxylic acid benzyl ester as a clear oil (3.5 g) which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06756372B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-42a59463843a4185bf3d936d002d28ef |
| Source note | uspto-grants-2004_06 |