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Magnesium bromide diethyl etherate → Phytanyl Bromide

HRID 1470216
ノート
印刷プレビュー

反応式

HRID 1470216 の反応式
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]
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 9903262Magnesium bromide diethyl etherateHCID 60047967Phytanyl Mesylate

生成物 1

HCID 10808570Phytanyl Bromide収率 90%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-7744767a1e73483e974f8e5baabed9c2
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09006417B2

反応ノート

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