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3,5-Dimethylisoxazole-4-sulfonyl chloride → HCID 19068786, 화합물

HRID 1957254
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HRID 1957254 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[C:14]([Cl:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][N:10]=2)[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:20][C:21]1[C:25]([S:26](Cl)(=[O:28])=[O:27])=[C:24]([CH3:30])[O:23][N:22]=1>C1(C)C=CC=CC=1.N1C=CC=CC=1>[Cl:8][C:7]1[CH:6]=[CH:5][C:4]([C:9]2[C:14]([Cl:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][N:10]=2)=[CH:3][C:2]=1[NH:1][S:26]([C:25]1[C:21]([CH3:20])=[N:22][O:23][C:24]=1[CH3:30])(=[O:28])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 27363193,5-Dimethylisoxazole-4-sulfonyl chlorideHCID 15766880HCID 15766880, 화합물

생성물 1

HCID 19068786HCID 19068786, 화합물수율 50.1%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 1140Toluene용매

실험 절차

A solution of 2.5 g of 2-(3-amino-4-chlorophenyl)-3-chloro-5-trifluoromethylpyridine and 2.3 g of 3,5-dimethylisoxazole-4-sulfonyl chloride in a mixture of 100 ml of toluene and 100 ml of pyridine was refluxed for 16 hours. The mixture was concentrated and the residue was taken up in 50 ml of ethyl acetate. The solution was washed with 50 ml each of 10% strength hydrochloric acid and 10% strength aqueous sodium bicarbonate solution and was dried over sodium sulfate and concentrated. Chromatography on silica gel with cyclohexane/ethyl acetate (6:1) resulted in 1.9 g of colorless crystals; melting point: 161°-162° C.

후처리

  1. temperaturewas refluxed for 16 hours
  2. concentrationThe mixture was concentrated
  3. washThe solution was washed with 50 ml each of 10% strength hydrochloric acid and 10% strength aqueous sodium bicarbonate solution
  4. dry with materialwas dried over sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-777a7276b9fe472fb762b8a01c884b7f
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05783522

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