Dimethyl Sulfoxide → 4-(5-Bromo-2-pyrimidinyloxy)-3-chloroaniline

HRID 4512

반응식

HRID 4512 반응식
[Br:1][C:2]1[CH:3]=[N:4][C:5](Cl)=[N:6][CH:7]=1.[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([Cl:17])[CH:11]=1.C(=O)([O-])[O-].[K+].[K+].CS(C)=O>O>[Br:1][C:2]1[CH:3]=[N:4][C:5]([O:16][C:13]2[CH:14]=[CH:15][C:10]([NH2:9])=[CH:11][C:12]=2[Cl:17])=[N:6][CH:7]=1

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 775784-Amino-2-chlorophenolHCID 6066655-Bromo-2-chloropyrimidine

생성물 1

HCID 137714404-(5-Bromo-2-pyrimidinyloxy)-3-chloroaniline수율 62.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a flask, 7.00 g of 5-bromo-2-chloropyrimidine, 5.19 g of 4-amino-2-chlorophenol, 9.98 g of potassium carbonate and 70 ml of dimethylsulfoxide were introduced, and reacted in a nitrogen atmosphere at 120° C. for 1.5 hours under stirring. After the completion of the reaction, the product was poured into water, and extracted with ethyl acetate. The extract was washed with water and a saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate, and then purified by silica gel column chromatography, whereby 6.80 g of oily 4-(5-bromo-2-pyrimidinyloxy)-3-chloroaniline was obtained.

후처리

  1. customreacted in a nitrogen atmosphere at 120° C. for 1.5 hours
  2. customAfter the completion of the reaction
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materiala saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate
  6. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-21579b9c6dbe424cb126459426052c6c
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727077

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