Triethylamine → 6-(2-chloropyrimidin-4-ylamino)-N,2-dimethylbenzofuran-3-carboxamide

HRID 16236노트

반응식

HRID 16236 반응식
CCN(CC)CC.[Cl:8][C:9]1[N:14]=[C:13](Cl)[CH:12]=[CH:11][N:10]=1.[NH2:16][C:17]1[CH:30]=[CH:29][C:20]2[C:21]([C:25]([NH:27][CH3:28])=[O:26])=[C:22]([CH3:24])[O:23][C:19]=2[CH:18]=1>CCO>[Cl:8][C:9]1[N:14]=[C:13]([NH:16][C:17]2[CH:30]=[CH:29][C:20]3[C:21]([C:25]([NH:27][CH3:28])=[O:26])=[C:22]([CH3:24])[O:23][C:19]=3[CH:18]=2)[CH:12]=[CH:11][N:10]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 775312,4-DichloropyrimidineHCID 597308036-amino-N,2-dimethylbenzofuran-3-carboxamide

생성물 1

HCID 592247466-(2-chloropyrimidin-4-ylamino)-N,2-dimethylbenzofuran-3-carboxamide수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Et3N (1 mmol) was added to a solution of 2,4-dichloropyrimidine (1 mmol) and 6-amino-N,2-dimethylbenzofuran-3-carboxamide (1 mmol) in 5 ml EtOH. The reaction mixture was refluxed for 5 hours. After removal of the solvent in vacuo and addition of H2O, the mixture was subjected to extraction with EtOAc. The organic layers were combined, washed with water and brine sequentially, dried over anhydrous Na2SO4, and concentrated in vacuo. The resulting residue was purified by column chromatography to give 6-(2-chloropyrimidin-4-ylamino)-N,2-dimethylbenzofuran-3-carboxamide in a yield of 80%.

후처리

  1. temperatureThe reaction mixture was refluxed for 5 hours
  2. customAfter removal of the solvent
  3. additionin vacuo and addition of H2O
  4. extractionthe mixture was subjected to extraction with EtOAc
  5. washwashed with water and brine sequentially
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe resulting residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-8c822fe44f9b48d29be898fc7bcb9c37
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737157B2

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