Hydrochloric Acid → 3,4-diethyl 1H-pyrazole-3,4-dicarboxylate

HRID 1958327

반응식

HRID 1958327 반응식
Cl.O.[NH2:3]N.Cl.[CH2:6]([O:8][C:9](=[O:22])[C:10](=[CH:18][N:19](C)C)[C:11](=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH3:7]>C(O)C>[CH2:15]([O:14][C:12]([C:11]1[NH:3][N:19]=[CH:18][C:10]=1[C:9]([O:8][CH2:6][CH3:7])=[O:22])=[O:13])[CH3:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 22250811Hydrazine monohydrate hydrochlorideHCID 72733183Diethyl 2-((dimethylamino)methylene)-3-oxosuccinate

생성물 1

HCID 145056993,4-diethyl 1H-pyrazole-3,4-dicarboxylate수율 31%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

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+].

후처리

  1. customThe solvent was evaporated
  2. washwashed (water)
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-b3bf88598dd54aedbaeccee6e6f5ec2f
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410117B2

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