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Acetyl chloride → 1-(4'-t-Butyldimethylsilyloxy-3'-methoxyphenyl)-1-hexene-3,5-dione

HRID 1650390
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HRID 1650390 반응식
[Si:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[CH:16][C:17](=[O:19])[CH3:18])=[CH:11][C:10]=1[O:20][CH3:21])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C([N-]C(C)C)(C)C.[Li+].[C:30](Cl)(=[O:32])[CH3:31].C(OCC)C.CCCCCC>C1COCC1>[Si:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[CH:16][C:17](=[O:19])[CH2:18][C:30](=[O:32])[CH3:31])=[CH:11][C:10]=1[O:20][CH3:21])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 6367Acetyl chlorideHCID 2724682Lithium diisopropylamideHCID 21584099Diethylether hexaneHCID 545292101-(4'-t-Butyldimethylsilyloxy-3'-methoxyphenyl)-1-butene-3-one

생성물 1

HCID 541564831-(4'-t-Butyldimethylsilyloxy-3'-methoxyphenyl)-1-hexene-3,5-dione수율 34.3%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

반응 조건

온도
-78 °C

실험 절차

A solution of 1-(4'-t-butyldimethylsilyloxy-3'-methoxyphenyl)-1-butene-3-one (12.8 g, 41.8 mmol) in THF (50 mL) is cooled to -78° C. under an argon atmosphere. Lithium di-isopropyl amide (83.5 mmol, in 50 mL THF) is slowly added to the reaction mixture. The reaction is stirred at -78° C. for 30 minutes. Acetyl chloride (16.4 g, 209 mmol) dissolved in THF (20 mL) is then added to the reaction over a 30 minute period. The reaction is quenched with aqueous HCl. The layers are separated, and the aqueous layer is washed with ethyl acetate. The combined organic layers are washed with saturated aqueous sodium bicarbonate, dried over MgSO4, and evaporated to give a red oil. Flash chromatography (ethyl ether/hexane 2:8) afford 5.0 g (34%) of 1-(4'-t-butyldimethylsilyloxy-3'-methoxyphenyl)-1-hexene-3,5-dione, mp=81°-85° C.

후처리

  1. additionis then added to the reaction over a 30 minute period
  2. customThe reaction is quenched with aqueous HCl
  3. customThe layers are separated
  4. washthe aqueous layer is washed with ethyl acetate
  5. washThe combined organic layers are washed with saturated aqueous sodium bicarbonate
  6. dry with materialdried over MgSO4
  7. customevaporated
  8. customto give a red oil

출처 및 근거

ORD 기록
ord-bd9c0fd87dc9417d9668c4d6379a675e
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04924002

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