Dimethylformamide → HCID 67325346、化合物

HRID 1616941

反応式

HRID 1616941 の反応式
[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

参加物

5

反応物 4

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

生成物 1

HCID 67325346HCID 67325346、化合物収率 37.8%

反応条件

温度
65 °C

実験手順

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]+.

後処理

  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)

出典と根拠

ORDレコード
ord-26b89431d05b4ac4a031f081e8aa30ca
出典データセット
uspto-grants-2014_07
特許番号
US08765779B2

関連ノート

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