Sodium Carbonate → HCID 66664995、化合物

HRID 607259ノート

反応式

HRID 607259 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)=[C:4]([N+:16]([O-])=O)[CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)(=O)C.C(O)C.O.[Fe]>[NH2:16][C:4]1[CH:3]=[C:2]([Cl:1])[CH:15]=[CH:14][C:5]=1[O:6][C:7]1[CH:8]=[CH:9][C:10]([OH:13])=[CH:11][CH:12]=1

参加物

7

反応物 2

HCID 10340Sodium CarbonateHCID 129406294-(4-Chloro-2-nitrophenoxy)phenol

生成物 1

HCID 66664995HCID 66664995、化合物収率 100%

試薬・触媒・溶媒 4

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of the product of Example 151A (400 mg, 1.506 mmol) and iron powder (336 mg, 6.02 mmol) in acetic acid (10 mL) and ethanol (10 mL) was heated at reflux under a nitrogen atmosphere for 25 minutes. The reaction was cooled to room temperature, diluted with water (50 mL), and treated with solid sodium carbonate until the pH was 6. Extracted with ethyl acetate (2×50 mL) and washed the organic with brine (50 mL), dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation under vacuum. Co-evaporating the resulting oil with methylene chloride/hexanes provided the title compound as a tan solid (355 mg, 100%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux under a nitrogen atmosphere for 25 minutes
  3. extractionExtracted with ethyl acetate (2×50 mL)
  4. washwashed the organic with brine (50 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by rotary evaporation under vacuum
  8. customCo-evaporating the resulting oil with methylene chloride/hexanes

出典と根拠

ORDレコード
ord-95cd7d7e354b442ab3cfbfedd8c542e4
出典データセット
uspto-grants-2011_03
特許番号
US07915411B2

反応ノート

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