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Pyridine → tert-Butyl(4-chlorobutoxy)dimethylsilane

HRID 363692
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HRID 363692 반응식
[C:1]([Si:5](Cl)([CH3:7])[CH3:6])([CH3:4])([CH3:3])[CH3:2].[Cl:9][CH2:10][CH2:11][CH2:12][CH2:13][OH:14].N1C=CC=CC=1>C1COCC1.[N+]([O-])([O-])=O.[Ag+]>[Si:5]([O:14][CH2:13][CH2:12][CH2:11][CH2:10][Cl:9])([C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:7])[CH3:6]
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참가 물질

6

반응물 3

HCID 1049PyridineHCID 135694-Chloro-1-butanolHCID 28928tert-Butyldimethylsilyl chloride

생성물 1

HCID 3382519tert-Butyl(4-chlorobutoxy)dimethylsilane

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 8028Tetrahydrofuran용매

실험 절차

t-Butylchlorodimethylsilane (8.3 g, 55 mmol) was added to a stirred mixture of 4-chlorobutanol (5.0 mL, 50 mmol), silver nitrate (12.8 g, 75.1 mmol), and pyridine (4.0 mL, 50 mmol) in 40 mL of dry THF. After 4 hr, the reaction mixture was filtered through Celite and evaporated to give a yellow oil. The material was purified by distillation to provide 4-chlorobutyl t-butyldimethylsilyl ether as a colorless oil (11 g, quantitative). To a solution of triphenylmethane (5.10 g, 20.8 mmol) in 25 mL of dry THF at -78° C., 13.1 mL (21 mmol) of 1.6M n-butyllithium was added dropwise under nitrogen. Shortly thereafter, 4.29 g (19.3 mmol) of 4-chlorobutyl t-butyldimethylsilyl ether was added. After addition of water and extraction with hexane, the product was purified by chromatography on silica gel with 1:3 dichloromethane-hexane, providing t-butyldimethylsilyl 5,5,5-triphenylpentyl ether as an oil (6.85 g). This material was dissolved in THF (30 mL) and 16 mL of 1.0M tetrabutylammonium fluoride in THF was added. After 3 hr, the mixture was acidified with 1N HCl, extracted with three portions of ethyl acetate, and the extracts dried over magnesium sulfate and evaporated in vacuo. The product was purified by chromatography on silica gel with a 10%-20% gradient of ethyl acetate in hexane, providing the title compound as a white solid, 3.83 g (63% overall).

후처리

  1. filtrationthe reaction mixture was filtered through Celite
  2. customevaporated
  3. customto give a yellow oil
  4. distillationThe material was purified by distillation

출처 및 근거

ORD 기록
ord-8398a87459ac4d03ad1891ec8923b437
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05874436

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