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Dimethyl Sulfoxide → 4-(4-Amino-3-chlorophenoxy)pyridin-2-ylamine

HRID 387822
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반응식

HRID 387822 반응식
[NH2:1][C:2]1[CH:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][C:11]=1[Cl:17].[H-].[Na+].CS(C)=O>O>[NH2:1][C:2]1[CH:7]=[C:6]([O:16][C:13]2[CH:14]=[CH:15][C:10]([NH2:9])=[C:11]([Cl:17])[CH:12]=2)[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 24758Sodium hydrideHCID 871844-Amino-3-chlorophenolHCID 5818662-Amino-4-chloropyridine

생성물 1

HCID 229367984-(4-Amino-3-chlorophenoxy)pyridin-2-ylamine수율 55.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The publicly known compound 2-amino-4-chloropyridine (5.0 g), 4-amino-3-chlorophenol (11 g), sodium hydride (60% in oil) (3.1 g) and dimethylsulfoxide (80 ml) were stirred at 160° C. for 9.5 hours. Water was added, extraction was performed with ethyl acetate, and the extract solution was washed 5 times with water. The extract solution was then passed through a glass filter coated with silica gel. The silica gel was washed with ethyl acetate, the ethyl acetate layers were combined, and the solvent was distilled off under reduced pressure to obtain 5.1 g of a dark violet solid.

후처리

  1. extractionextraction
  2. washthe extract solution was washed 5 times with water
  3. filtrationfilter
  4. washThe silica gel was washed with ethyl acetate
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-4161df7ccaf943da891f541e85c64f9f
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372981B2

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