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Methylamine → N-Methyl-1-(p-tolyl)-5-(4-chlorophenyl)-1H-pyrazole-3-carboxamide

HRID 55358
ノート
印刷プレビュー

反応式

HRID 55358 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=3)=[CH:11][C:10]([C:20](Cl)=[O:21])=[N:9]2)=[CH:4][CH:3]=1.C(Cl)Cl.[CH3:26][NH2:27]>C(O)C>[CH3:26][NH:27][C:20]([C:10]1[CH:11]=[C:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)[N:8]([C:5]2[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][CH:4]=2)[N:9]=1)=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6329MethylamineHCID 6344DichloromethaneHCID 54331566HCID 54331566、化合物

生成物 1

HCID 19957364N-Methyl-1-(p-tolyl)-5-(4-chlorophenyl)-1H-pyrazole-3-carboxamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 0.50 g of 1-(4-methylphenyl)-5-(4-chlorophenyl)pyrazole-3-carboxylic acid chloride in ml of CH2Cl2 is added dropwise to 100 ml of a 33% solution of methylamine in ethanol. After stirring for hours at room temperature, the mixture is concentrated under vacuum, the residue is taken up with a mixture of 5% Na2CO3 +AcOEt, the organic phase is decanted, washed with a saturated solution of NaCl and dried over MgSO4 and the solvents are evaporated off. The residue is taken up in isopropyl ether and the crystals obtained are filtered off and dried under vacuum to give 0.44 g of the expected amide.

後処理

  1. concentrationthe mixture is concentrated under vacuum
  2. additionthe residue is taken up with a mixture of 5% Na2CO3 +AcOEt
  3. customthe organic phase is decanted
  4. washwashed with a saturated solution of NaCl
  5. dry with materialdried over MgSO4
  6. customthe solvents are evaporated off
  7. customthe crystals obtained
  8. filtrationare filtered off
  9. customdried under vacuum

出典と根拠

ORDレコード
ord-8de981eb7b8446c1be8ea774e7329d62
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05624941

反応ノート

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