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Allyl bromide → HCID 67266810, 화합물

HRID 1698291
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HRID 1698291 반응식
C(=O)([O-])O.[Na+].[CH2:6]([O:11][C:12]1[C@@H:17]([C@H:18]([CH2:20][OH:21])[OH:19])[O:16][C:14](=[O:15])[C:13]=1[OH:22])[CH:7]([CH2:9][OH:10])[OH:8].[CH2:23](Br)[CH:24]=[CH2:25]>O>[CH2:6]([O:11][C:12]1[C@@H:17]([C@H:18]([CH2:20][OH:21])[OH:19])[O:16][C:14](=[O:15])[C:13]=1[O:22][CH2:25][CH:24]=[CH2:23])[CH:7]([CH2:9][OH:10])[OH:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 516892Sodium BicarbonateHCID 672677953-Glyceryl ascorbate

생성물 1

HCID 67266810HCID 67266810, 화합물수율 152.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Under an argon atmosphere, water and sodium hydrogen carbonate (1.42 g) were added to 3-O-glyceryl ascorbic acid (1.42 g) obtained in Example 1, and the mixture was stirred at room temperature for 30 minutes. To the mixture, allyl bromide (2.45 g) was added, and the resultant mixture was heated up to 60° C. and stirred for 2 hours. Thereafter, the mixture was concentrated under reduced pressure, then, dissolved in methanol. Then, the resultant solution was dried over anhydrous sodium sulfate, and concentrated under reduced pressure, and 6.70 g of the resultant residue was subjected to silica gel column chromatography. Elution was performed with chloroform/methanol/water(volume ratio:10/3/0.4), and concentration was performed under reduced pressure to obtain to obtain 3-O-glyceryl-2-O-allyl ascorbic acid (2.51 g).

후처리

  1. stirringstirred for 2 hours
  2. concentrationThereafter, the mixture was concentrated under reduced pressure
  3. dissolutiondissolved in methanol
  4. dry with materialThen, the resultant solution was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure, and 6.70 g of the resultant residue
  6. washElution
  7. concentrationwas performed with chloroform/methanol/water(volume ratio:10/3/0.4), and concentration
  8. customto obtain

출처 및 근거

ORD 기록
ord-90570c7389324e139b19d5fbb0187655
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163939B2

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