Water → HCID 20077451、化合物

HRID 1655022ノート

反応式

HRID 1655022 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[CH:8][C:9](=[O:13])[NH:10]2)=[CH:5][CH:4]=1.[H-].[Na+].[CH3:22]I.O>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[CH:8][C:9](=[O:13])[N:10]2[CH3:22])=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 7227187-methoxy-4-phenyl-quinolin-2-ol

生成物 1

HCID 20077451HCID 20077451、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

A solution of 7-methoxy-4-phenyl-2-quinolinone from Example 1, Step 2 (1.62 g) in DMF (30 mL) was treated with NaH (60% in mineral oil; 310 mg). After stirring at 50° C. for 45 min., the mixture was cooled to r.t. and methyl iodide (0.6 mL) was added. After 30 min., H2O (100 mL) was added and the resulting solution extracted with EtOAc (3×). The organics were washed with H2O (2×), brine, dried (MgSO4) and the solvents evaporated. Flash chromatography of the residue (silica gel; CHCl3 /EtOAc (4:1)) provided the title compound as a foam.

後処理

  1. temperaturethe mixture was cooled to r.t.
  2. waitAfter 30 min.
  3. extractionthe resulting solution extracted with EtOAc (3×)
  4. washThe organics were washed with H2O (2×), brine
  5. dry with materialdried (MgSO4)
  6. customthe solvents evaporated

出典と根拠

ORDレコード
ord-c8004835cb9f40c5a304476917eda2f1
出典データセット
uspto-grants-1995_04
特許番号
US05410054

反応ノート

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