Sodium Carbonate → HCID 66664995, 화합물

HRID 607259노트

반응식

HRID 607259 반응식
[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

참가 물질

7

반응물 2

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

생성물 1

HCID 66664995HCID 66664995, 화합물수율 100%

시약·촉매·용매 4

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-95cd7d7e354b442ab3cfbfedd8c542e4
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915411B2

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