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Acetic Acid → HCID 25155178、化合物

HRID 2405164
ノート
印刷プレビュー

反応式

HRID 2405164 の反応式
[CH2:1]([O:17][CH2:18][CH:19]([CH2:29][OH:30])[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]([OH:28])CO)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].C(O)(=O)C>C(O)(C)C.O.C(O)C.C[N+](CC(NN)=O)(C)C.[Cl-]>[CH2:1]([O:17][CH2:18][CH:19]([CH2:29][OH:30])[O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH:25]=[O:28])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

HCID 176Acetic AcidHCID 25155177HCID 25155177、化合物

生成物 1

HCID 25155178HCID 25155178、化合物収率 27%

試薬・触媒・溶媒 4

HCID 67156Girard-T reagent触媒HCID 702Ethanol溶媒HCID 962Water溶媒3 回
HCID 3776
Isopropanol
溶媒

実験手順

As depicted in Scheme III, 1-Hexadecyl-2-(5′,6′-dihydroxy-hexanyl)-glycerol (7.84 grams) was dissolved in isopropanol (50 ml) and water (12 ml). NaIO4 (9 grams) was added and the reaction mixture was stirred at room temperature for 3 hours. Water (50 ml) was added and the reaction mixture extracted with chloroform (3×50 ml), dried over anhydrous Na2SO4, filtered and the solvent removed under reduced pressure yielding 5.56 grams. The crude product was dissolved in ethanol (60 ml) and glacial acetic acid (2.3 grams). Girard's reagent T (5.6 grams) was added and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled in ice-bath, alkaline solution (2.3 grams in 45 ml water) was added and the mixture was extracted with ether (3×25 ml). The etheral phase was washed with water and the water combined with the alkaline phase. The aqueous phase was acidified with concentrated HCl (4.4 ml) and extracted with ether (3×25 ml). Washing with water, saturated aqueous sodium bicarbonate (3×25 ml), water (2×25 ml), drying over anhydrous Na2SO4 and removal of the solvent under reduced pressure gave 1.95 grams (0.0049 mol) of 1-Hexadecyl-2-(5′-oxo-pentanyl)-glycerol (26.9% yield).

後処理

  1. extractionthe reaction mixture extracted with chloroform (3×50 ml)
  2. dry with materialdried over anhydrous Na2SO4
  3. filtrationfiltered
  4. customthe solvent removed under reduced pressure
  5. customyielding 5.56 grams
  6. temperaturethe reaction mixture was refluxed for 2 hours
  7. temperatureThe reaction mixture was cooled in ice-bath
  8. extractionthe mixture was extracted with ether (3×25 ml)
  9. washThe etheral phase was washed with water
  10. extractionextracted with ether (3×25 ml)
  11. washWashing with water, saturated aqueous sodium bicarbonate (3×25 ml), water (2×25 ml)
  12. dry with materialdrying over anhydrous Na2SO4 and removal of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-629991cc2a844c0089959d872081217d
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08802875B2

反応ノート

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