참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Hydrazine monohydrate hydrochloride | HCID 22250811 | — |
| 반응물 | Diethyl 2-((dimethylamino)methylene)-3-oxosuccinate | HCID 72733183 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 3,4-diethyl 1H-pyrazole-3,4-dicarboxylate | HCID 14505699 | 31% |
반응 단계
Under an atmosphere of argon, hydrazine monohydrate hydrochloride (1.91 g, 28 mmol) and HCl (36.5% in water, 2.8 ml) were added to a solution of 2-dimethylaminomethylene-3-oxo-succinic acid diethyl ester (6.8 g, 28 mmol) in ethanol (100 ml). The mixture was heated to 60° C. (3 h). The solvent was evaporated, and the residue was taken up in dichloromethane and washed (water). The organic layer was dried (Na2SO4), the solvent was evaporated and the title compound (1.81 mg, 31%) was isolated from the mixture by column chromatography (silica gel, heptane:ethyl acetate=100:0-60:40). MS (m/e)=383.3 [M+H+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08410117B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_04 |
|---|
| ORD ID | ord-b3bf88598dd54aedbaeccee6e6f5ec2f |
|---|
| 출처 메모 | uspto-grants-2013_04 |
|---|
