Dimethylformamide → HCID 22674164, 화합물

HRID 1173139노트

반응식

HRID 1173139 반응식
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[Br:12].Cl[C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][N:15]=1.CN(C)C=O.[CH3:29][S-:30].[Na+]>[Cl-].[Na+].O.N1C=CC=CC=1>[Br:12][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[N:4]=[CH:3][C:2]([NH:1][S:20]([C:17]1[CH:18]=[CH:19][C:14]([S:30][CH3:29])=[N:15][CH:16]=1)(=[O:22])=[O:21])=[CH:11]2

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 27927922-Chloro-5-pyridinesulfonyl chlorideHCID 4378561Sodium methanethiolateHCID 226741618-Bromoquinolin-3-amine

생성물 1

HCID 22674164HCID 22674164, 화합물수율 27%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 57417360Sodium chloride; water용매

실험 절차

197 mg (0.556 mmol) of white crystals were obtained using 100 mg (0.56 mmol, Production Example 5b) of 3-amino-8-bromoquinoline and 142 mg (0.67 mmol) of 2-chloro-5-pyridinesulfonyl chloride in the same manner as in Synthetic Example 1b. Dimethylformamide (1 ml), pyridine (1 ml) and 111 mg (1.6 mmol) of sodium thiomethoxide were added to 60 mg (0.17 mmol) of the crystals, followed by stirring at room temperature for 3 hours. Brine was added to the reaction solution, followed by extracting with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated, to give the residue. The residue was purified by silica gel chromatography, to give 62 mg of the title compound.

후처리

  1. extractionby extracting with ethyl acetate
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customto give the residue
  5. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-9cc8a4e4094943219b9ad84b901a812f
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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