HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → tert-Butyl 2,4-dioxopiperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | tert-Butyl (3-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)-3-oxopropyl)carbamate | HCID 68556020 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | tert-Butyl 2,4-dioxopiperidine-1-carboxylate | HCID 23730999 | 83% |
Reaction Conditions
| Temperature | 105 °C |
|---|
Reaction Steps
Tert-butyl 3-(2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)-3-oxopropylcarbamate (I-59b: 50 g, 158.57 mmol) was dissolved in ethyl acetate (500 mL) at room temperature under nitrogen atmosphere and the resulting reaction mass was heated at 105° C. for 20 hours. The reaction was monitored by TLC (10% methanol in DCM). The reaction mass was cooled to room temperature and concentrated under reduced pressure to afford the crude product. Purification by ether-wash afforded 28 g of the product (83% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946260B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-d523c2a6945b4779912a904dc9b44fb0 |
| Source note | uspto-grants-2015_02 |