Dimethylformamide → HCID 67325346, 화합물

HRID 1616941

반응식

HRID 1616941 반응식
[I:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([OH:8])[CH:7]=1.Br[CH:11]([CH3:13])[CH3:12].C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>>[I:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([O:9][CH:11]([CH3:13])[CH3:12])[CH:3]=1

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 63582-BromopropaneHCID 11430Potassium CarbonateHCID 6167555-Iodobenzene-1,3-diol

생성물 1

HCID 67325346HCID 67325346, 화합물수율 37.8%

반응 조건

온도
65 °C

실험 절차

A mixture of 5-Iodo-benzene-1,3-diol (2 g, 8 mmol), 2-bromopropane (0.88 mL, 9.3 mmol) and potassium carbonate (1.3 g, 9.3 mmol) in DMF (15 mL, 190 mmol) was stirred at 65° C. After 18 h, the mixture was cooled to RT and the solvent was evaporated. The residue was dissolved in DCM, washed with water and brine. The solvent was evaporated and the residue was purified on silica gel using an ISCO instrument and eluting with hexanes:EtOAc (4:1) to afford the title product (841 mg). MS m/z: 279 [M+H]+.

후처리

  1. temperaturethe mixture was cooled to RT
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in DCM
  4. washwashed with water and brine
  5. customThe solvent was evaporated
  6. customthe residue was purified on silica gel using an ISCO instrument
  7. washeluting with hexanes:EtOAc (4:1)

출처 및 근거

ORD 기록
ord-26b89431d05b4ac4a031f081e8aa30ca
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765779B2

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