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Sodium Bicarbonate → HCID 11780000、化合物

HRID 574264
ノート
印刷プレビュー

反応式

HRID 574264 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 67144432HCID 67144432、化合物

生成物 1

HCID 11780000HCID 11780000、化合物収率 63%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e46c22891c644344a5fad821716819f3
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034850B2

反応ノート

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