Pyridine → 2-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide

HRID 53519

반응식

HRID 53519 반응식
[NH2:1][C:2]1[C:3]([Cl:9])=[N:4][CH:5]=[CH:6][C:7]=1[CH3:8].[Cl:10][C:11]1[N:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13](Cl)=[O:14].N1C=CC=CC=1.C1CCCCC1>O1CCOCC1>[Cl:10][C:11]1[C:12]([C:13]([NH:1][C:2]2[C:3]([Cl:9])=[N:4][CH:5]=[CH:6][C:7]=2[CH3:8])=[O:14])=[CH:16][CH:17]=[CH:18][N:19]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8078CyclohexaneHCID 27563873-Amino-2-chloro-4-methylpyridineHCID 27745412-Chloronicotinoyl chloride

생성물 1

HCID 104238682-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide수율 4.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Using a procedure analogous to that described in Example 1a, the carboxamide was prepared from 12.8 g of 3-amino-2-chloro-4-methyl pyridine, 15.8 g of 2-chloronicotinoyl chloride, 7.1 g of pyridine, 30 ml of cyclohexane and 60 ml of dioxane. After removal of the solvent, the product was dissolved in methylene chloride, washed with water and dried (sodium sulfate). After removal of the solvent, the residue was washed with ethyl acetate to give 1.2 g of the title compound, m.p. 193°-194° C.

후처리

  1. customAfter removal of the solvent
  2. dissolutionthe product was dissolved in methylene chloride
  3. washwashed with water
  4. dry with materialdried (sodium sulfate)
  5. customAfter removal of the solvent
  6. washthe residue was washed with ethyl acetate

출처 및 근거

ORD 기록
ord-347bb4d39b864da4bcaa306b0d10cdd3
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620974

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