Trimethoxysilane → 1-Nitro-2-[[[6-(trimethoxysilyl)hexyl]oxy]methyl]benzene

HRID 2216233

반응식

HRID 2216233 반응식
[N+:1]([C:4]1[CH:17]=[CH:16][CH:15]=[CH:14][C:5]=1[CH2:6][O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]=[CH2:13])([O-:3])=[O:2].[CH3:18][O:19][SiH:20]([O:23][CH3:24])[O:21][CH3:22]>[H+].[H+].O.O.O.O.O.O.Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl>[CH3:18][O:19][Si:20]([O:23][CH3:24])([O:21][CH3:22])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][O:7][CH2:6][C:5]1[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=1[N+:1]([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 17215TrimethoxysilaneHCID 219410445-Hexenyl 2-nitrobenzyl ether

생성물 1

HCID 219410341-Nitro-2-[[[6-(trimethoxysilyl)hexyl]oxy]methyl]benzene수율 52%

시약·촉매·용매 1

HCID 134756Platinic chloride hexahydrate촉매

반응 조건

온도
37 °C

실험 절차

A 20-ml eggplant type flask was purged with nitrogen, and charged with 2.5 g (10.7 mmol) of 5-hexenyl 2-nitrobenzyl ether, 1.56 g (12.8 mmol) of trimethoxysilane, and an infinitesimal amount of hydrogen hexachloroplatinate(IV) hexahydrate (H2PtCl6·6H2O), followed by stirring at 37° C. for 30 minutes. Thereafter, the bath temperature was raised to 100° C., and the reaction was completed in 2 hours. After the temperature was returned to room temperature, the reaction mixture was purified by vacuum distillation using a short path. From the second fraction (0.2 mmHg/123–125° C.), 1.98 g of the desired product was obtained in a 52% yield.

후처리

  1. customA 20-ml eggplant type flask was purged with nitrogen
  2. temperatureThereafter, the bath temperature was raised to 100° C.
  3. waitthe reaction was completed in 2 hours
  4. customwas returned to room temperature
  5. distillationthe reaction mixture was purified by vacuum distillation

출처 및 근거

ORD 기록
ord-2d9155c759fb4b829b13bde5566b9088
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112397B2

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