Dimethylformamide → HCID 22674164, 화합물

HRID 1005696노트

반응식

HRID 1005696 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

White crystals (197 mg, 0.556 mmol) were obtained in the same manner as in Example 1, except using 100 mg (0.56 mmol) of 3-amino-8-bromoquinoline (Preparation Example 5) and 142 mg (0.67 mmol) of 2-chloro-5-pyridinesulfonyl chloride. To the crystals (60 mg, 0.17 mmol) were added dimethylformamide (1 ml), pyridine (1 ml) and sodium thiomethoxide (111 mg, 1.6 mmol), followed by stirring at room temperature for 3 hours. TO the reaction mixture was added brine, followed by extracting with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated. The resulting 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. customThe resulting residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-f631e972daf34bb6bbcf6e5d0df22fa4
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787534B2

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