Iodine → HCID 178440467、化合物

HRID 14501ノート

反応式

HRID 14501 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9](=[O:24])[C:10]3[C:11]([O:19][C:20]=2[CH:21]([CH3:23])[CH3:22])=[C:12]2[C:16](=[CH:17][CH:18]=3)[NH:15][N:14]=[CH:13]2)=[CH:4][CH:3]=1.[OH-].[K+].[I:27]I>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9](=[O:24])[C:10]3[C:11]([O:19][C:20]=2[CH:21]([CH3:22])[CH3:23])=[C:12]2[C:16](=[CH:17][CH:18]=3)[NH:15][N:14]=[C:13]2[I:27])=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 807IodineHCID 14797Potassium HydroxideHCID 687032613-(4-Chlorophenyl)-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one

生成物 1

HCID 178440467HCID 178440467、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-(4-chlorophenyl)-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one (20 mg, 0.059 mmol) in dry N,N-dimethylformamide (2 ml) at room temperature are added potassium hydroxide (6.3 mg, 0.112 mmol) and iodine (55 mg, in three portions over 3 h, 0.217 mmol). The reaction mixture is stirred at room temperature for 20 h, then diluted with ethyl acetate and washed successively with 10% aqueous sodium thiosulfate solution (40 ml) and saturated brine (40 ml). The organic phase is dried (MgSO4), filtered and evaporated under reduced pressure. The resulting solid is triturated with n-hexane/dichloromethane to give a colourless solid that is recovered by filtration and dried.

後処理

  1. washwashed successively with 10% aqueous sodium thiosulfate solution (40 ml) and saturated brine (40 ml)
  2. dry with materialThe organic phase is dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe resulting solid is triturated with n-hexane/dichloromethane
  6. customto give a colourless solid that
  7. filtrationis recovered by filtration
  8. customdried

出典と根拠

ORDレコード
ord-008d1b1039134b6bb27ddee169105178
出典データセット
uspto-grants-2010_06
特許番号
US07732435B2

反応ノート

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