Triethoxysilane → 2-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(4-triethoxysilanylbutyloxy)benzoate

HRID 1739493노트

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HRID 1739493 반응식
[CH2:1]([O:5][C:6]1[CH:28]=[CH:27][C:9]([C:10]([O:12][C:13]2[CH:18]=[CH:17][C:16](/[CH:19]=[CH:20]/[C:21]([O:23][CH3:24])=[O:22])=[CH:15][C:14]=2[O:25][CH3:26])=[O:11])=[CH:8][CH:7]=1)[CH2:2][CH:3]=[CH2:4].[CH2:29]([O:31][SiH:32]([O:36][CH2:37][CH3:38])[O:33][CH2:34][CH3:35])[CH3:30]>C([Si](C=C)(C)O[Si](C)(C)C)=C.[Pt].C1(C)C=CC=CC=1>[CH2:29]([O:31][Si:32]([O:36][CH2:37][CH3:38])([O:33][CH2:34][CH3:35])[CH2:4][CH2:3][CH2:2][CH2:1][O:5][C:6]1[CH:28]=[CH:27][C:9]([C:10]([O:12][C:13]2[CH:18]=[CH:17][C:16](/[CH:19]=[CH:20]/[C:21]([O:23][CH3:24])=[O:22])=[CH:15][C:14]=2[O:25][CH3:26])=[O:11])=[CH:8][CH:7]=1)[CH3:30]

참가 물질

5

반응물 2

HCID 13830Triethoxysilane2회HCID 218413722-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(3-butenyloxy)benzoate

생성물 1

HCID 218412092-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(4-triethoxysilanylbutyloxy)benzoate

시약·촉매·용매 2

HCID 86614225Platinum divinyltetramethyldisiloxane촉매HCID 1140Toluene용매

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온도
60 °C

실험 절차

Air was conducted for 30 min. into a mixture of 1 g of 2-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(3-butenyloxy)benzoate, 0.480 ml of triethoxysilane, 10 ml of toluene and 0.017 ml of platinum divinyltetramethyldisiloxane (3-3.5% in toluene) and the mixture was then stirred at 60° C. for 1 hr. Then, a further 0.1 ml of triethoxysilane was added and the mixture was left to react at 60° C. for 16 hrs. The reaction mixture was thereafter cooled to room temperature and partitioned between ethyl acetate and water. The organic phase was thereupon dried over magnesium sulphate, filtered and evaporated to dryness. Chromatography on 150 g of silica gel with toluene/ethyl acetate (19:1 to 9:1) gave 0.60 g of 2-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(4-triethoxysilanylbutyloxy)benzoate as a colorless liquid, λmax. (CH2Cl2): 279 nm.

후처리

  1. waitthe mixture was left
  2. customto react at 60° C. for 16 hrs
  3. temperatureThe reaction mixture was thereafter cooled to room temperature
  4. custompartitioned between ethyl acetate and water
  5. dry with materialThe organic phase was thereupon dried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-d2945cece13f4c8ba2f92c02530eb2f9
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05965761

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