Iodine → HCID 178440467, 화합물

HRID 14501노트

반응식

HRID 14501 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 178440467HCID 178440467, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-008d1b1039134b6bb27ddee169105178
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

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