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1,5-Diazabicyclo(4.3.0)non-5-ene → HCID 178490723、化合物

HRID 2241169
ノート
印刷プレビュー

反応式

HRID 2241169 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:31][CH3:32])=[C:6]([S:8]([NH:11][C:12]2[CH:13]=[C:14]([CH:28]=[CH:29][CH:30]=2)[C:15]([NH:17][C:18]2[CH:23]=[CH:22][C:21]([C:24](=[NH:27])[NH:25][OH:26])=[CH:20][CH:19]=2)=[O:16])(=[O:10])=[O:9])[CH:7]=1.[C:33](N1C=CN=C1)(N1C=CN=C1)=[S:34].N12CCCC1=NCCC2>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:31][CH3:32])=[C:6]([S:8]([NH:11][C:12]2[CH:13]=[C:14]([CH:28]=[CH:29][CH:30]=2)[C:15]([NH:17][C:18]2[CH:19]=[CH:20][C:21]([C:24]3[NH:27][C:33](=[S:34])[O:26][N:25]=3)=[CH:22][CH:23]=2)=[O:16])(=[O:10])=[O:9])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 802641,1'-ThiocarbonyldiimidazoleHCID 1784907253-(5-chloro-2-methoxy-benzenesulfonylamino)-N-[4-(N-hydroxycarbamimidoyl)-phenyl]-benzamide

生成物 1

HCID 178490723HCID 178490723、化合物収率 20.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

3-(5-Chloro-2-methoxy-benzenesulfonylamino)-N-[4-(N-hydroxycarbamimidoyl)-phenyl]-benzamide (110 mg, 0.23 mmol) was diluted in acetonitrile (2 ml) under argon. 1,1′-Thiocarbonyldiimidazole (TCDI) (68 mg, 0.38 mmol, 1.65 equiv.) was then added, followed by 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) (114 mg, 3.95 equiv.). The mixture was stirred at room temperature for 6 hours, then the solvents were evaporated. The residue was diluted with water and the pH was adjusted to 4 with HCl 1N. The aqueous phase was extracted with ethyl acetate, and the organic phase evaporated. The residue was dissolved in NaOH 1N, and washed with ether. The aqueous solution was adjusted to pH 4 with HCl 1N and then extracted with ethyl acetate. The organic phase was dried over sodium sulfate and evaporated. Purification via flash chromatography (dichloromethane/methanol) yielded the title compound as a light yellow solid (24 mg, 20%), MS (ISP): m/e=515.1 (M−H).

後処理

  1. customthe solvents were evaporated
  2. additionThe residue was diluted with water
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. customthe organic phase evaporated
  5. dissolutionThe residue was dissolved in NaOH 1N
  6. washwashed with ether
  7. extractionextracted with ethyl acetate
  8. dry with materialThe organic phase was dried over sodium sulfate
  9. customevaporated
  10. customPurification via flash chromatography (dichloromethane/methanol)

出典と根拠

ORDレコード
ord-8deadd2ab1e94fd9b6d285c17665510b
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07723538B2

反応ノート

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