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Tetrahydrofuran → 2-(1,3,5-Triethylphenyl)-2-oxoacetic acid

HRID 579245
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HRID 579245 반응식
O1CCCC1.[CH2:6]([C:8]1([C:18](=[O:24])[C:19]([O:21]CC)=[O:20])[CH:13]=[C:12]([CH2:14][CH3:15])[CH:11]=[C:10]([CH2:16][CH3:17])[CH2:9]1)[CH3:7].[OH-].[Na+]>O>[CH2:6]([C:8]1([C:18](=[O:24])[C:19]([OH:21])=[O:20])[CH:9]=[C:10]([CH2:16][CH3:17])[CH:11]=[C:12]([CH2:14][CH3:15])[CH2:13]1)[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 66691385Ethyl 2-(1,3,5-triethylphenyl)-2-oxoacetate

생성물 1

HCID 666915612-(1,3,5-Triethylphenyl)-2-oxoacetic acid수율 92.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 3 L volume four-necked flask, tetrahydrofuran (750 ml) and ethyl 2-(1,3,5-triethylphenyl)-2-oxoacetate (9-b) (261.0 g) were added, and sodium hydroxide (88 g) dissolved in water (237 g) was added dropwise thereto at about 15-20° C. The resulting mixture was stirred at room temperature for 1 hour and 30 minutes. The solid was removed by decantation. The liquid part was concentrated under reduced pressure. The residue was extracted with toluene and water. After the organic layer was removed, the aqueous layer was washed with toluene. The pH of the aqueous layer was adjusted to 1 with dilute sulfuric acid under cooling, and then the aqueous layer was extracted with toluene. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and filtered to remove the insolubles. The filtrate was concentrated under reduced pressure to give 214.8 g of 2-(1,3,5-triethylphenyl)-2-oxoacetic acid (8-b).

후처리

  1. additionwas added dropwise
  2. customat about 15-20° C
  3. customThe solid was removed by decantation
  4. concentrationThe liquid part was concentrated under reduced pressure
  5. extractionThe residue was extracted with toluene and water
  6. customAfter the organic layer was removed
  7. washthe aqueous layer was washed with toluene
  8. temperatureunder cooling
  9. extractionthe aqueous layer was extracted with toluene
  10. washThe organic layer was washed with water
  11. dry with materialdried over anhydrous magnesium sulfate
  12. filtrationfiltered
  13. customto remove the insolubles
  14. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3719a0bdef014c9ebd265148913bd5e4
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040709B2

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