Acetonitrile → HCID 23154178、化合物

HRID 639443ノート

反応式

HRID 639443 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 23154178HCID 23154178、化合物収率 41.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a76bd133696a42cbab395e41794e2c15
出典データセット
uspto-grants-2010_04
特許番号
US07691860B2

反応ノート

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