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tert-Butyldimethylsilyl chloride → HCID 19385687, 화합물

HRID 2399486
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HRID 2399486 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[OH:12])[C:5]([O:7][CH3:8])=[O:6].[C:13]([Si:17]([CH3:20])([CH3:19])Cl)([CH3:16])([CH3:15])[CH3:14]>C(Cl)Cl.CN(C)C1C=CN=CC=1>[Si:17]([O:12][C:11]1[CH:10]=[CH:9][C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:3][C:2]=1[Cl:1])([C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 28928tert-Butyldimethylsilyl chlorideHCID 77580Methyl 3-chloro-4-hydroxybenzoate

생성물 1

HCID 19385687HCID 19385687, 화합물수율 100%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 5.00 g (26.8 mmol) of methyl 3-chloro-4-hydroxybenzoate dissolved in 40 mL of CH2Cl2 was added 6.55 g (53.6 mmol) of 4-dimethylaminopyridine, 4.85 g (32.2 mmol) of tert-butyldimethylchlorosilane and the mixture was stirred at room temperature for 3.5 hours. The reaction mixture was filtered, diluted with ethyl acetate, washed with 0.1N HCl, saturated NaHCO3, and brine. The product layer was then dried (MgSO4), filtered and evaporated in vacuo to afford 8.05 g (100%) of the title compound.

후처리

  1. filtrationThe reaction mixture was filtered
  2. additiondiluted with ethyl acetate
  3. washwashed with 0.1N HCl, saturated NaHCO3, and brine
  4. dry with materialThe product layer was then dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-f039a8f718c6490caeb744571025ea7d
출처 데이터셋
uspto-grants-1995_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05449682

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