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Water → HCID 86665236、化合物

HRID 1028080
ノート
印刷プレビュー

反応式

HRID 1028080 の反応式
[CH2:1]([OH:21])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20].[OH-:22].[Na+].[OH2:24].[C:25]1([CH3:31])[CH:30]=CC=C[CH:26]=1>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:1]([O:21][C:25]([CH3:26])([CH3:31])[C:30]([O:24][C:25]([CH3:31])([CH3:30])[CH3:26])=[O:22])[CH2:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1140TolueneHCID 14798Sodium HydroxideHCID 59539494(5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol

生成物 1

HCID 86665236HCID 86665236、化合物収率 44%

試薬・触媒・溶媒 1

HCID 70681Tetrabutylammonium Chloride
触媒

実験手順

A mixture of (5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol, (0.83 g, 3.14 mmol), tetrabutylammonium chloride (0.24 g, 0.85 mmol) and t-butyl α-bromo isobutyrate (3.50 g, 15.7 mmol) was dissolved in toluene (15 mL) and placed under nitrogen. An aqueous solution of sodium hydroxide (50%, 5 mL) was added slowly under vigorous stirring at room temperature. The resulting mixture was heated to 60° C. and stirred for six hours. The mixture was cooled, added water and extracted three times with ether. The combined organic extract was washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography on silica gel using a gradient of 5-10% ethyl acetate in heptane as eluent. Concentration of the appropriate fractions afforded 0.60 g (44% yield) of the title compound as an oil. MS (electro spray): 453.3 [M+Na]+.

後処理

  1. temperatureThe resulting mixture was heated to 60° C.
  2. stirringstirred for six hours
  3. temperatureThe mixture was cooled
  4. extractionextracted three times with ether
  5. extractionThe combined organic extract
  6. washwas washed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe residue was purified by flash chromatography on silica gel using a gradient of 5-10% ethyl acetate in heptane as eluent

出典と根拠

ORDレコード
ord-2536c05290894130931798c4ec299952
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735436B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート