HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Aminoacetanilide → 4-(3-Acetylamino-phenylamino)-piperidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Aminoacetanilide | HCID 7604 | — |
| Reactant | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 4-(3-Acetylamino-phenylamino)-piperidine-1-carboxylic acid tert-butyl ester | HCID 67400739 | 49% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of N-(3-amino-phenyl)-acetamide (0.19 g, 1.25 mmol, 1.0 equiv; commercially available) and 4-oxo-piperidine-1-carboxylic acid tert-butyl ester (0.3 g, 1.50 mmol, 1.2 equiv; commercially available) in isopropanol (2 mL) was heated by microwave irradiation to 120° C. for 20 min. Sodium cyanoborohydride (0.16 g, 2.50 mmol, 2.0 equiv), dissolved in isopropanol (2 mL), was added and the reaction mixture heated by microwave irradiation to 120° C. for an additional time period of 20 min. The crude reaction material was purified by silica column chromatography eluting with heptane/ethyl acetate (1:2) providing 0.21 g (49%) of the title compound. MS (ISP): 334.3 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07754744B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-529132d3b2cb4f888680857a030ca548 |
| Source note | uspto-grants-2010_07 |