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Magnesium bromide diethyl etherate → Phytanyl Bromide

HRID 537819
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HRID 537819 반응식
CCOCC.[Mg+2].[Br-:7].[Br-].S(O[CH2:14][CH2:15][CH:16]([CH2:18][CH2:19][CH2:20][CH:21]([CH2:23][CH2:24][CH2:25][CH:26]([CH2:28][CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH3:27])[CH3:22])[CH3:17])(=O)(=O)C>C(OCC)C>[CH2:14]([Br:7])[CH2:15][CH:16]([CH2:18][CH2:19][CH2:20][CH:21]([CH2:23][CH2:24][CH2:25][CH:26]([CH2:28][CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH3:27])[CH3:22])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9903262Magnesium bromide diethyl etherateHCID 60047967Phytanyl Mesylate

생성물 1

HCID 10808570Phytanyl Bromide수율 90%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension of magnesium bromide diethyl etherate (25.9 g, 100.3 mmol) in anhydrous diethyl ether (250 mL) under nitrogen at room temperature was added a solution of phytanyl mesylate (18.9 g, 50.2 mmol) in anhydrous diethyl ether (200 mL) dropwise over 15 minutes. The resulting slurry was stirred for 72 hours at room temperature. Upon completion, the reaction mixture was cooled to 0° C. and ice cold water was added dropwise until all solid dissolved and bubbling stopped. Diethyl ether (300 mL) was added, and the organic and aqueous layers separated. The aqueous layer was back-extracted with diethyl ether (200 mL). The combined diethyl ether extracts were dried on MgSO4, filtered, and concentrated. The resulting oil was purified by column chromatography (column 10″L×2″W; eluted with 100% hexanes) to afford the product as a pale yellow oil (16.3 g, 90%).

후처리

  1. temperatureUpon completion, the reaction mixture was cooled to 0° C.
  2. additionice cold water was added dropwise until all solid
  3. dissolutiondissolved
  4. custombubbling
  5. additionDiethyl ether (300 mL) was added
  6. customthe organic and aqueous layers separated
  7. extractionThe aqueous layer was back-extracted with diethyl ether (200 mL)
  8. dry with materialThe combined diethyl ether extracts were dried on MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe resulting oil was purified by column chromatography (column 10″L×2″W; eluted with 100% hexanes)

출처 및 근거

ORD 기록
ord-c79d6af0c51b458096e518832148653f
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865675B2

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