Hydrochloric Acid → Ethyl 3-aminopyridazine-4-carboxylate

HRID 2217966노트

반응식

HRID 2217966 반응식
[NH2:1][C:2]1[N:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]([OH:10])=[O:9].Cl.[C:12]1(C)C=CC(S(Cl)(=O)=O)=C[CH:13]=1>C(O)C>[CH2:12]([O:9][C:8]([C:7]1[CH:6]=[CH:5][N:4]=[N:3][C:2]=1[NH2:1])=[O:10])[CH3:13]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 64052513-Amino-4-pyridazinecarboxylic acid

생성물 1

HCID 68940790Ethyl 3-aminopyridazine-4-carboxylate수율 1,163.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-Aminopyridazine-4-carboxylic acid (1.68 g, prepared as in JOC, (1985), 50, 346) was refluxed in ethanol (170 ml) with concentrated hydrochloric acid (2 ml) and p-toluene-sulphonyl chloride (0.1 g) for 55 hours. The solvent was evaporated and ice water added to the residue, which was then neutralised with solid sodium bicarbonate. The mixture was extracted with chloroform, insoluble material filtered, the organic extract dried over magnesium sulphate and evaporated to give 3-aminopyridazine-4-carboxylic acid ethyl ester (1.02 g) as a white solid.

후처리

  1. customThe solvent was evaporated
  2. additionice water added to the residue, which
  3. extractionThe mixture was extracted with chloroform, insoluble material
  4. filtrationfiltered
  5. extractionthe organic extract
  6. dry with materialdried over magnesium sulphate
  7. customevaporated

출처 및 근거

ORD 기록
ord-5002fe2692d8471cab97158222e24642
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07410967B2

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