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Sodium Bicarbonate → HCID 11780000, 화합물

HRID 574264
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HRID 574264 반응식
[C:1]([Si:5]([CH3:24])([CH3:23])[O:6][C@H:7]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:8][O:9][Si](C(C)(C)C)(C)C)([CH3:4])([CH3:3])[CH3:2].C(=O)(O)[O-].[Na+]>CO>[C:1]([Si:5]([CH3:24])([CH3:23])[O:6][CH:7]([C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[CH2:8][OH:9])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 67144432HCID 67144432, 화합물

생성물 1

HCID 11780000HCID 11780000, 화합물수율 63%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of [(R)-1,2-bis-(tert-butyl-dimethyl-silanyloxy)-ethyl]-benzene (625 mg, 1.7 mmol) in methanol (3 mL) was slowly added ferric chloride III) (276 mg, 1.7 mmol) with stirring at room temperature. When the reaction was monitored to be completed about 25 min after the addition, an aqueous saturated sodium bicarbonate solution was added. The solution was extracted with ethyl ether and the organic layer thus formed was separated. To the organic layer was added sodium sulfate, followed by stirring for 5 min and filtering. The filtrate was concentrated and dried in a vacuum, and the residue was purified using silica gel chromatography (eluent: hexane/ethyl acetate, 16/1) and dried in a vacuum to afford 270 mg of the compound as a colorless oil (yield 63%).

후처리

  1. additionafter the addition
  2. extractionThe solution was extracted with ethyl ether
  3. customthe organic layer thus formed
  4. customwas separated
  5. additionTo the organic layer was added sodium sulfate
  6. stirringby stirring for 5 min
  7. filtrationfiltering
  8. concentrationThe filtrate was concentrated
  9. customdried in a vacuum
  10. customthe residue was purified
  11. customdried in a vacuum

출처 및 근거

ORD 기록
ord-e46c22891c644344a5fad821716819f3
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09034850B2

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