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5-Chloro-4-(6-chloro-3'-fluoro-4-(pyridazin-4-yl)biphenyl-3-yloxy)-N-(2,4-dimethoxybenzyl)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide → 5-Chloro-4-[(6-chloro-3'-fluoro-4-pyridazin-4-ylbiphenyl-3-yl)oxy]-2-fluoro-N-1,3,4-thiadiazol-2-ylbenzenesulfonamide

HRID 1619616
ノート
印刷プレビュー

反応式

HRID 1619616 の反応式
[Cl:1][C:2]1[C:3]([O:29][C:30]2[CH:31]=[C:32]([C:43]3[CH:48]=[CH:47][CH:46]=[C:45]([F:49])[CH:44]=3)[C:33]([Cl:42])=[CH:34][C:35]=2[C:36]2[CH:41]=[CH:40][N:39]=[N:38][CH:37]=2)=[CH:4][C:5]([F:28])=[C:6]([S:8]([N:11](CC2C=CC(OC)=CC=2OC)[C:12]2[S:13][CH:14]=[N:15][N:16]=2)(=[O:10])=[O:9])[CH:7]=1>Cl.O1CCOCC1>[Cl:1][C:2]1[C:3]([O:29][C:30]2[CH:31]=[C:32]([C:43]3[CH:48]=[CH:47][CH:46]=[C:45]([F:49])[CH:44]=3)[C:33]([Cl:42])=[CH:34][C:35]=2[C:36]2[CH:41]=[CH:40][N:39]=[N:38][CH:37]=2)=[CH:4][C:5]([F:28])=[C:6]([S:8]([NH:11][C:12]2[S:13][CH:14]=[N:15][N:16]=2)(=[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

4

反応物 1

HCID 580422475-Chloro-4-(6-chloro-3'-fluoro-4-(pyridazin-4-yl)biphenyl-3-yloxy)-N-(2,4-dimethoxybenzyl)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide

生成物 1

HCID 580423205-Chloro-4-[(6-chloro-3'-fluoro-4-pyridazin-4-ylbiphenyl-3-yl)oxy]-2-fluoro-N-1,3,4-thiadiazol-2-ylbenzenesulfonamide収率 63.3%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

5-Chloro-4-(6-chloro-3′-fluoro-4-(pyridazin-4-yl)biphenyl-3-yloxy)-N-(2,4-dimethoxybenzyl)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide (Preparation 97, 60 mg, 0.08 mmol) was dissolved in a 4M solution of HCl in dioxane (5 mL). The reaction was stirred for 18 hours at room temperature and then evaporated in vacuo. The residue was dissolved in ethyl acetate (5 mL) washed with water (2×5 mL), dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography eluting with dichloromethane:methanol:acetic acid (97:2.7:0.3) to give 30 mg of the title compound. The compound was further purified by preparative HPLC to give the title compound (3.6 mg, 7.5%) as a solid.

後処理

  1. customevaporated in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate (5 mL)
  3. washwashed with water (2×5 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography
  8. washeluting with dichloromethane:methanol:acetic acid (97:2.7:0.3)

出典と根拠

ORDレコード
ord-2de8ccfc23dc4830948df18c971491f2
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772293B2

反応ノート

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