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

HRID 1739493ノート

反応式

HRID 1739493 の反応式
[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]

参加物

5

反応物 2

HCID 13830Triethoxysilane2 回HCID 218413722-methoxy-4-[(E)2-methoxycarbonyl-vinyl]phenyl 4-(3-butenyloxy)benzoate

生成物 1

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

試薬・触媒・溶媒 2

HCID 86614225Platinum divinyltetramethyldisiloxane触媒HCID 1140Toluene溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d2945cece13f4c8ba2f92c02530eb2f9
出典データセット
uspto-grants-1999_10
特許番号
US05965761

反応ノート

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