Hydrochloric Acid → Ethyl 3-aminopyridazine-4-carboxylate

HRID 2217966ノート

反応式

HRID 2217966 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 68940790Ethyl 3-aminopyridazine-4-carboxylate収率 1,163.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5002fe2692d8471cab97158222e24642
出典データセット
uspto-grants-2008_08
特許番号
US07410967B2

反応ノート

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