Acetonitrile → HCID 23154178, 화합물

HRID 639443노트

반응식

HRID 639443 반응식
C(#N)C.[O:4]=[S:5]1(=[O:16])[CH2:9][CH2:8][CH2:7][N:6]1[CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[CH3:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([N:28]2[C:32]3[CH:33]=[CH:34][C:35]([C:37]4[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=4)=[CH:36][C:31]=3[N:30]=[C:29]2Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1.C(N(C(C)C)CC)(C)C>C(OCC)(=O)C.O>[O:16]=[S:5]1(=[O:4])[CH2:9][CH2:8][CH2:7][N:6]1[CH:10]1[CH2:15][CH2:14][N:13]([C:29]2[N:28]([S:25]([C:22]3[CH:21]=[CH:20][C:19]([O:18][CH3:17])=[CH:24][CH:23]=3)(=[O:27])=[O:26])[C:32]3[CH:33]=[CH:34][C:35]([C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)=[CH:36][C:31]=3[N:30]=2)[CH2:12][CH2:11]1

참가 물질

7

반응물 4

HCID 6342AcetonitrileHCID 81531DiisopropylethylamineHCID 23154167HCID 23154167, 화합물HCID 532560872-(piperidin-4-yl)-1lambda6,2-thiazolidine-1,1-dione

생성물 1

HCID 23154178HCID 23154178, 화합물수율 41.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To the acetonitrile solution (3 mL) containing 4-(1,1-dioxo-1λ6-isothiazolidin-2-yl)piperidine (136 mg) were added 1-(4-methoxyphenylsulfonyl)-2-chloro-5-phenylbenzimidazole (340 mg) and diisopropylethylamine (0.41 mL), followed by stirring at room temperature for 16 hrs. The reaction mixture was diluted with ethyl acetate and water, and the organic layer was washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was separated and purified on a collective thin-layer chromatograph (ethyl acetate) to give the title compound (157 mg).

후처리

  1. washthe organic layer was washed with an aqueous saturated sodium chloride solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was separated
  5. custompurified on a collective thin-layer chromatograph (ethyl acetate)

출처 및 근거

ORD 기록
ord-a76bd133696a42cbab395e41794e2c15
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691860B2

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