1,4-Dioxane → HCID 22504414, 화합물

HRID 1432246

반응식

HRID 1432246 반응식
C[Si]([C:5]#[C:6][C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1)(C)C.[C:13]1([S:19]([NH:22][C:23]2[C:28](I)=[CH:27][C:26]([S:30]([CH3:33])(=[O:32])=[O:31])=[CH:25][CH:24]=2)(=[O:21])=[O:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C([O-])(=O)C.[K+].O1CCOCC1>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(OCC)(=O)C.O>[C:13]1([S:19]([N:22]2[C:23]3[C:24](=[CH:25][C:26]([S:30]([CH3:33])(=[O:32])=[O:31])=[CH:27][CH:28]=3)[CH:5]=[C:6]2[C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)(=[O:20])=[O:21])[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

8

반응물 4

HCID 312751,4-DioxaneHCID 517044Potassium AcetateHCID 41008573-(Trimethylsilylethynyl)pyridineHCID 225043761-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene

생성물 1

HCID 22504414HCID 22504414, 화합물수율 63%

시약·촉매·용매 3

HCID 178418476HCID 178418476, 화합물촉매HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

A mixture of 3-trimethylsilylethynylpyridine (1.07 g), 2-benzenesulfonylamino-3-iodo-5-methanesulfonylbenzene (1.75 g), potassium acetate (1.60 g), cuprous iodide (60 mg), dichlorobis(triphenylphosphine)palladium (0.20 g) and 1,4-dioxane (4 ml) was stirred at 100° C. for 12 hours under nitrogen atmosphere. To the reaction solution were added water and ethyl acetate. The insolubles were filtered off. The filtrate was extracted with ethyl acetate, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (hexane:ethyl acetate=1:3) to obtain 1.04 g of the desired product.

후처리

  1. filtrationThe insolubles were filtered off
  2. extractionThe filtrate was extracted with ethyl acetate
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6e4de20a21ef493895c8a9c5532b031c
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612070B2

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