Sodium Hydroxide → 1-(4-Ethynylphenyl)ethan-1-one

HRID 1095234노트

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HRID 1095234 반응식
C[C:2]1[C:3](C)=[C:4]([C:11]#[C:12]CO)[CH:5]=[CH:6][C:7]=1[C:8](=[O:10])[CH3:9].[OH-].[Na+]>C1(C)C=CC=CC=1>[C:8]([C:7]1[CH:6]=[CH:5][C:4]([C:11]#[CH:12])=[CH:3][CH:2]=1)(=[O:10])[CH3:9]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 66784133HCID 66784133, 화합물

생성물 1

HCID 51236261-(4-Ethynylphenyl)ethan-1-one수율 56%

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
120 °C

실험 절차

1.45 g (7.17 mmol) of dimethylhydroxymethyl-4-acetylphenylacetylene and 301 mg (7.53 mmol) of NaOH (KISHIDA CHEMICAL CO., Ltd., 0.7 mm granular, 98%) were placed in a 100 mL two-neck flask equipped with a reflux condenser and the air inside the flask was replaced with Ar. 36 mL of toluene was added thereto and the mixture was refluxed at 120° C. for 15 minutes. Toluene was added to the reaction mixture and the mixture was washed with a saturated aqueous ammonium chloride solution and dried over magnesium sulfate, followed by distilling off of the solvent under reduced pressure by an evaporator. Then, 25 mL of hexane was added to the resulting crude reaction product and the mixture was cooled to give 4-acetylphenylethyne as a yellow solid. (0.74 g, yield: 56%).

후처리

  1. customequipped with a reflux condenser
  2. washthe mixture was washed with a saturated aqueous ammonium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. distillationby distilling off of the solvent under reduced pressure by an evaporator
  5. additionThen, 25 mL of hexane was added to the resulting crude
  6. customreaction product
  7. temperaturethe mixture was cooled

출처 및 근거

ORD 기록
ord-51a39bf682344d698bde5af78593cdee
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08137821B2

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