Dimethylformamide → HCID 22459155、化合物

HRID 2185030ノート

反応式

HRID 2185030 の反応式
FC1(C2C=CC=C([O:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([O:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[CH:22][C:21]=3[CH2:33][CH2:34][CH3:35])C=2)SC(=O)NC1=O.O([C:43]1[CH:48]=[CH:47][C:46](O)=[C:45]([CH2:50][CH2:51]C)[CH:44]=1)C1C=CC=CC=1.[C:53](=O)([O-])[O-:54].[Cs+].[Cs+].CN(C=[O:63])C>>[CH2:33]([C:21]1[CH:22]=[C:23]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:24]=[CH:25][C:20]=1[O:19][CH2:18][CH2:17][CH2:16][O:15][C:48]1[CH:43]=[CH:44][C:45]([CH2:50][C:51]([O:54][CH3:53])=[O:63])=[CH:46][CH:47]=1)[CH2:34][CH3:35]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 9848632HCID 9848632、化合物HCID 154629044-Phenoxy-2-propylphenol

生成物 1

HCID 22459155HCID 22459155、化合物

実験手順

A solution of the product from Step A (11.0 g, 38.58 mmol), 4-phenoxy-2-propylphenol (PCT Application WO97/28115; 8.0 g, 35.07 mmol) and cesium carbonate (12.0 g, 36.82 mmol) in DMF (80 mL) was stirred at 40° C. overnight. The reaction mixture was partitioned between ethyl acetate and 0.2N HCl. The organic layer was washed twice with water, then dried over sodium sulfate. The organic layer was filtered and evaporated to an oil which was chromatographed over silica gel with 10% of ethyl acetate in hexane to afford the title compound.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and 0.2N HCl
  2. washThe organic layer was washed twice with water
  3. dry with materialdried over sodium sulfate
  4. filtrationThe organic layer was filtered
  5. customevaporated to an oil which
  6. customwas chromatographed over silica gel with 10% of ethyl acetate in hexane

出典と根拠

ORDレコード
ord-bdc8da64ba1745abb1a7d2c80f586e1b
出典データセット
uspto-grants-2002_06
特許番号
US06399640B1

反応ノート

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