Triethylamine → N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide

HRID 704317

반응식

HRID 704317 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([O:8][C:9]2[CH:15]=[CH:14][C:12]([NH2:13])=[CH:11][C:10]=2[CH3:16])=[N:6][CH:7]=1.C(N(CC)CC)C.[N+:24]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[S:33]Cl)([O-:26])=[O:25].C(OCC)(=O)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[N:6][C:5]([O:8][C:9]2[CH:15]=[CH:14][C:12]([NH:13][S:33][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=3[N+:24]([O-:26])=[O:25])=[CH:11][C:10]=2[CH3:16])=[N:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 243192-Nitrobenzenesulfenyl chlorideHCID 142078084-((5-Chloropyrimidin-2-yl)oxy)-3-methylaniline

생성물 1

HCID 10000368N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide수율 83.6%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

2.0 g of 4-(5 chloro-2-pyrimidinyloxy)-3methylaniline and 0.94 g of triethylamine were dissolved in 20 ml of toluene, and a solution of 1.61 g of 2-nitrobenzenesulfenyl chloride dissolved in 5 ml of toluene was dropwise added thereto at room temperature. The mixture was reacted at room temperature for 1 hour under stirring. After completion of the reaction, ethyl acetate was added to the reaction product, and the ethyl acetate layer was washed with water, dried over Glauber's salt and then purified by column chromatography to obtain 2.76 g of N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide (Intermediate Compound No. 37) (melting point: 74°-85° C.) in a yellow non-crystalline form.

후처리

  1. additionwas dropwise added
  2. customat room temperature
  3. customThe mixture was reacted at room temperature for 1 hour
  4. additionwas added to the reaction product
  5. washthe ethyl acetate layer was washed with water
  6. dry with materialdried over Glauber's salt
  7. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-635377d9a71e459093799c5dc60a7731
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987135

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