HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 84653985, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ethyl 1-ethyl-4,5-dioxopyrrolidine-3-carboxylate | HCID 219264 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 84653985 | HCID 84653985 | 71.5% |
Reaction Steps
A solution of ethyl 1-ethyl-4,5-dioxopyrrolidine-3-carboxylate (150 mg, 0.753 mmol) and LiOH (43.3 mg, 1.81 mmol) in THF (0.5 mL) and H2O (0.5 mL) was heated at 80° C. for 1 h using microwave irradiation. The reaction solution was concentrated under reduced pressure and acidified with 1 N aqueous HCl, whereupon a precipitate formed. CH2Cl2 was added to the suspension and the precipitate was collected by filtration and dried in vacuo to provide Intermediate 8 (92.1 mg, 71.4% yield). HPLC/MS (Method D) RT=0.48 min, [M+H]+ 172.1; 1H NMR (400 MHz, Solvent) (δ ppm): 1.11-1.24 (m, 3H), 3.53 (q, J=7.28 Hz, 2H), 3.84 (s, 0.47H), 4.04 (s, 1.53H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249096B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-8d083a6f10194ba6a6735a700fea174d |
| Source note | uspto-grants-2016_02 |