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Aluminum(III) Chloride → HCID 19047070, 화합물

HRID 1780614
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HRID 1780614 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Al+3].[Cl-].[Cl-].[Cl-].[CH3:11][C:12]1([CH3:25])[CH2:16][C:15]2[C:17]([CH3:24])=[C:18]([CH:22]=O)[CH:19]=[C:20]([CH3:21])[C:14]=2[O:13]1>C(OCC)C>[CH3:11][C:12]1([CH3:25])[CH2:16][C:15]2[C:17]([CH3:24])=[C:18]([CH3:22])[CH:19]=[C:20]([CH3:21])[C:14]=2[O:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6451240Aluminum(III) Chloride2회HCID 19047059HCID 19047059, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19047070HCID 19047070, 화합물수율 88.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension of 9.75 g of lithium aluminum hydride in 200 ml of absolute diethyl ether was added 34.27 g of AlCl3 and added dropwise a mixture of 42 g of the 2,3-dihydro-2,2,4,7-tetramethylbenzofuran-5-carboxaldehyde and 27.4 g of AlCl3 in 100 ml of absolute diethyl ether. After stirring for 30 minutes, the reaction mixture was quenched with 10 ml of ethyl acetate and added with 100 ml of water and 100 ml of 2N aqueous solution of hydrochloric acid. The organic extract was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to afford a crude product. Final purification was carried by vacuum distillation to afford 34.5 g of 2,3-dihydro-2,2,4,5,7-pentamethylbenzofuran as colorless oil.

후처리

  1. additionadded dropwise
  2. customthe reaction mixture was quenched with 10 ml of ethyl acetate
  3. additionadded with 100 ml of water and 100 ml of 2N aqueous solution of hydrochloric acid
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto afford a crude product
  9. customFinal purification
  10. distillationwas carried by vacuum distillation

출처 및 근거

ORD 기록
ord-732d31f969a24baaafd92a31af1a9ef9
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05631208

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