Potassium Hydroxide → HCID 90103465, 화합물

HRID 1051392노트

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HRID 1051392 반응식
[OH-].[K+].[CH2:3]([O:5][C:6](=[O:17])[CH2:7][CH:8]([CH2:13][N+]([O-])=O)[C:9]([F:12])([F:11])[F:10])[CH3:4].[O-:18]S([O-])(=O)=O.[Mg+2].[O-][Mn](=O)(=O)=O.[K+]>C1COCC1.O>[CH2:3]([O:5][C:6](=[O:17])[CH2:7][CH:8]([CH:13]=[O:18])[C:9]([F:12])([F:11])[F:10])[CH3:4]

참가 물질

7

반응물 4

HCID 14797Potassium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 268363Ethyl 4,4,4-trifluoro-3-(nitromethyl)butanoateHCID 516875Potassium Permanganate

생성물 1

HCID 90103465HCID 90103465, 화합물

시약·촉매·용매 2

HCID 962Water용매3회HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

In a 100 mL round-bottomed flask, KOH (356 mg, 5.45 mmol) was combined with H2O (50 ml) to give a colorless solution and cooled to 0° C. 4,4,4-Trifluoro-3-nitromethyl-butyric acid ethyl ester (1.25 g, 5.45 mmol) in 10 ml THF was added and the resulting reaction mixture was stirred for 20 min. This was followed by addition of MgSO4 (657 mg, 5.45 mmol) in 5 ml of H2O then by KMnO4 (862 mg, 5.45 mmol) in 30 ml of H2O. The resulting reaction mixture was stirred for 30 min, filtered through celite and the celite cake washed with CH2Cl2. The combined filtrate and washes were washed with brine, dried over Na2SO4, filtered and concentrated to afford 4,4,4-trifluoro-3-formyl-butyric acid ethyl ester as a liquid which was used without purification.

후처리

  1. customto give a colorless solution
  2. customthe resulting reaction mixture
  3. customThe resulting reaction mixture
  4. stirringwas stirred for 30 min
  5. filtrationfiltered through celite
  6. washthe celite cake washed with CH2Cl2
  7. washThe combined filtrate and washes were washed with brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-955962637e704064a17b9764098c1f08
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388172B2

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