Triethylamine → 3-Acryloyloxypropyltriphenylsilane

HRID 1252241

반응식

HRID 1252241 반응식
[OH:1][CH2:2][CH2:3][CH2:4][Si:5]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:31](Cl)(=[O:34])[CH:32]=[CH2:33]>C1C=CC=CC=1>[C:31]([O:1][CH2:2][CH2:3][CH2:4][Si:5]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)(=[O:34])[CH:32]=[CH2:33]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 40603353-(Triphenylsilyl)propan-1-ol

생성물 1

HCID 141418833-Acryloyloxypropyltriphenylsilane수율 87.3%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

32.9 g (91.4 mmol) of compound (C) was added to a 1 N solution of sodium carbonate in ethanol and the mixture was heated at 70° to 80° C. for 3 h to conduct the hydrolysis. 27.7 g (87.1 mmol) of 3-hydroxypropyltriphenylsilane (D) was thus obtained (yield: 95.4%). 250 ml of dry benzene was placed in a flask after replacing air in the flask with a dry inert gas (argon). 5.0 g (15.7 mmol) of compound (D) and 1.9 g of triethylamine were dissolved therein. 50 ml of a solution of 1.6 g (17.7 mmol) of acryloyl chloride in benzene was added slowly thereto. After the completion of the addition, the mixture was stirred at room temperature for 6 h. The reaction solution was washed with a 0.5 N hydrochloric acid, water, a 1 N sodium carbonate solution and water successively and then dried over magnesium sulfate. Benzene was distilled off and the residue was purified according to column chromatography (silica gel/benzene) to obtain 5.1 g (13.7 mmol) of 3-acryloyloxypropyltriphenylsilane in the form of white crystals (yield: 87.3%).

후처리

  1. additionAfter the completion of the addition
  2. washThe reaction solution was washed with a 0.5 N hydrochloric acid, water
  3. dry with materiala 1 N sodium carbonate solution and water successively and then dried over magnesium sulfate
  4. distillationBenzene was distilled off
  5. customthe residue was purified

출처 및 근거

ORD 기록
ord-947d9dcd3993426a8bd166dc010d2995
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742136

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