Sodium Hydroxide → HCID 57706373, 화합물

HRID 1662518노트

반응식

HRID 1662518 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:25])=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([C:14](OC)=[O:15])=[CH:10][C:9]=2[C:18]2[C:22]([CH3:24])([CH3:23])[CH2:21][CH2:20][CH:19]=2)[CH:7]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>C1COCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:25])=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][OH:15])=[CH:10][C:9]=2[C:18]2[C:22]([CH3:23])([CH3:24])[CH2:21][CH2:20][CH:19]=2)[CH:7]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 57706006Methyl 5'-chloro-2-(5,5-dimethyl-1-cyclopenten-1-yl)-2'-fluoro-1,1'-biphenyl-4-carboxylate

생성물 1

HCID 57706373HCID 57706373, 화합물수율 63.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 78.9A (0.082 g, 0.23 mmol) in THF (5.00 mL) at 0° C. was added LAH (0.46 mL, 0.46 mmol, 1.0M). The reaction was then stirred for 1.5 hours. 1N NaOH(aq) was then added to the quench the reaction. The reaction was extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was purified on silica gel (0-20% EtOAc in hexanes) to yield 78.9B as a colorless oil (0.048 g, 63% yield).

후처리

  1. customquench
  2. customthe reaction
  3. extractionThe reaction was extracted three times with EtOAc
  4. dry with materialAfter drying over anhydrous magnesium sulfate
  5. filtrationfiltering
  6. customthe organic solvent was removed under reduced pressure
  7. customthe product was purified on silica gel (0-20% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-3461c1161d9f4be7812f8081b85d9791
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030354B2

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