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| | 1-Ethyl-2,3-dioxopiperazine Basic information |
| | 1-Ethyl-2,3-dioxopiperazine Chemical Properties |
| Melting point | 106-110 °C(lit.) | | Boiling point | 259.72°C (rough estimate) | | density | 0.64 | | refractive index | 1.5010 (estimate) | | storage temp. | Sealed in dry,Room Temperature | | solubility | 2000 g/L | | form | Solid | | pka | 12.57±0.20(Predicted) | | color | White to Off-White | | Water Solubility | 2000 g/L | | BRN | 879076 | | Major Application | pharmaceutical | | InChI | InChI=1S/C6H10N2O2/c1-2-8-4-3-7-5(9)6(8)10/h2-4H2,1H3,(H,7,9) | | InChIKey | ZBEKOEYCWKIMGU-UHFFFAOYSA-N | | SMILES | N1(CC)CCNC(=O)C1=O | | CAS DataBase Reference | 59702-31-7(CAS DataBase Reference) |
| Hazard Codes | Xi | | Risk Statements | 36/37/38 | | Safety Statements | 26-36-37 | | WGK Germany | 3 | | RTECS | TL6380250 | | HS Code | 29339900 | | Storage Class | 11 - Combustible Solids | | Hazard Classifications | Eye Irrit. 2
Skin Irrit. 2
STOT SE 3 |
| | 1-Ethyl-2,3-dioxopiperazine Usage And Synthesis |
| Chemical Properties | 1-Ethyl-2,3-dioxopiperazine is WHITE TO PALE YELLOW CRYSTALLINE POWDER | | Uses | 1-Ethyl-2,3-dioxopiperazine is an intermediate used in the new process for the synthesis of Piperacillin sodium. | | Uses | 1-Ethyl-2,3-dioxopiperazine (Piperacillin EP Impurity E; Piperacillin USP Related Compound E) is an intermediate used in the new process for the synthesis of Piperacillin sodium. | | Synthesis | A. Prepare Mixed Solution A by dissolving 11 g of N-ethyl ethylenediamine in 8 g of anhydrous methanol.B. Add 25 ml of anhydrous methanol to a dry three-necked flask and 2 g of glacial acetic acid under stirring, and when it is completely dissolved, 11 g of diethyl oxalate was slowly added at 25-30 °C, and the temperature of the reaction system was subsequently lowered to 15-20 °C. This mixed solution was transferred to a dropping funnel and set aside.C. Mixed Solution A was slowly added dropwise to Mixed Solution B, keeping the reaction temperature between 30-50 °C for 30-50 min. After the reaction was completed, the temperature was raised to 50°C and the reaction was continued for 1 hour. At the end of the reaction, methanol was removed by concentration under reduced pressure.D. 66 ml of solvent B was added to the reaction mixture and the temperature of the system was slowly lowered from 50 °C to room temperature (25-30 °C) to allow the product to crystallize slowly. Finally 14.77 g of N-ethyl-2,3-dioxopiperazine was obtained in 83.21% yield and 99.32% purity. | | References | [1] Patent: CN107417630, 2017, A. Location in patent: Paragraph 0017-0041 |
| | 1-Ethyl-2,3-dioxopiperazine Preparation Products And Raw materials |
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