4-Chlorophenol → HCID 15482077、化合物

HRID 380242ノート

反応式

HRID 380242 の反応式
[H-].[Na+].Cl[C:4]1[C:5]2[CH:14]=[C:13]3[O:15][CH2:16][O:17][C:12]3=[CH:11][C:6]=2[S:7][C:8]=1[CH:9]=[O:10].[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=1>CN(C)C=O>[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][C:4]2[C:5]3[CH:14]=[C:13]4[O:15][CH2:16][O:17][C:12]4=[CH:11][C:6]=3[S:7][C:8]=2[CH:9]=[O:10])=[CH:21][CH:20]=1

参加物

5

反応物 3

HCID 46844-ChlorophenolHCID 24758Sodium hydrideHCID 17820729HCID 17820729、化合物

生成物 1

HCID 15482077HCID 15482077、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1 equivalent of sodium hydride and then 0.094 mol of the product obtained in Step D are added at ambient temperature and under an inert atmosphere to a solution of 0.10 mol of 4-chlorophenol in 250 ml of dimethylformamide. After 12 hours' reaction at 80° C., the reaction mixture is concentrated under reduced pressure. The residue is then diluted with ethyl acetate, washed with water and then with an aqueous solution of NaOH and then of NaCl, dried over calcium sulphate, filtered and concentrated under reduced pressure. Chromatography over silica gel (dichloromethane/ethyl acetate: 98/2) allows the expected product to be isolated.

後処理

  1. customAfter 12 hours' reaction at 80° C.
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. additionThe residue is then diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialwith an aqueous solution of NaOH and then of NaCl, dried over calcium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto be isolated

出典と根拠

ORDレコード
ord-45198605680e4fbd866bbf6b8ae69d1d
出典データセット
uspto-grants-2001_10
特許番号
US06302837B1

反応ノート

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