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Methanol → HCID 21835981, 화합물

HRID 1417114
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HRID 1417114 반응식
[CH2:1]([Si:4]([CH2:14][CH:15]=[CH2:16])([CH2:11][CH:12]=[CH2:13])[CH2:5][CH2:6][CH2:7][O:8]C=O)[CH:2]=[CH2:3].CO.C(=O)([O-])O.[K+]>O>[CH2:14]([Si:4]([CH2:1][CH:2]=[CH2:3])([CH2:11][CH:12]=[CH2:13])[CH2:5][CH2:6][CH2:7][OH:8])[CH:15]=[CH2:16]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 516893Potassium BicarbonateHCID 53937165HCID 53937165, 화합물

생성물 1

HCID 21835981HCID 21835981, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

The triallyl formyloxypropyl silane intermediate was converted to the hydroxylpropyl product by charging 5.0 grams of the intermediate, together with 50 ml of methanol (commercially available from Burdick and Jackson of Muskeegon, Mich.) and 10 ml of deionized water, in a 250 ml flask with stir bar. 1.0 gram (10 millimoles) of potassium hydrogen carbonate (commercially available from Aldrich Chemical Co.) was added to the solution, which was then stirred at 50° C. for five hours. The solution was filtered and was concentrated in vacuo. The sample was then taken up in cyclohexane and was washed with saturated aqueous sodium chloride before drying over anhydrous sodium sulfate (commercially available from Aldrich Chemical Co.). The sample was then purified using flash chromatography on silica with 99/1 cyclohexane/acetone eluent initially, followed by 80/20 cyclohexane/acetone. The recovered fractions were concentrated in vacuo to yield triallyl 3-hydroxypropyl silane, as shown by capillary GC/FID analysis using a 30 meter DB-5 column. Spectroscopic analysis using mass spectrometry, FTIR and NMR was consistent with triallyl-3-hydroxypropyl silane.

후처리

  1. addition) was added to the solution, which
  2. filtrationThe solution was filtered
  3. concentrationwas concentrated in vacuo
  4. washwas washed with saturated aqueous sodium chloride
  5. dry with materialbefore drying over anhydrous sodium sulfate (commercially available from Aldrich Chemical Co
  6. customThe sample was then purified
  7. concentrationThe recovered fractions were concentrated in vacuo

출처 및 근거

ORD 기록
ord-128802f4420f4a7bac44b47d8415f7bf
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05876595

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