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Sodium hydride → (1R,5S,6S,7R)-3,3-Ethylenedioxy-7-benzoyloxy-6-[(4RS)-2-bromo-4-methyl-3-oxooct-1-en-6-ynyl]bicyclo[3.3.0]octane

HRID 466594
ノート
印刷プレビュー

反応式

HRID 466594 の反応式
COP([CH2:7][C:8](=[O:15])[CH:9]([CH3:14])[CH2:10][C:11]#[C:12][CH3:13])(=O)OC.[H-].[Na+].[Br:18]N1C(=O)CCC1=O.[CH2:26]1[CH2:48][O:47][C:28]2([CH2:35][C@H:34]3[C@H:30]([CH2:31][C@@H:32]([O:38][C:39](=[O:46])[C:40]4[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=4)[C@@H:33]3[CH:36]=O)[CH2:29]2)[O:27]1.[Cl-].[NH4+]>C(COC)OC>[CH2:26]1[CH2:48][O:47][C:28]2([CH2:35][C@H:34]3[C@H:30]([CH2:31][C@@H:32]([O:38][C:39](=[O:46])[C:40]4[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=4)[C@@H:33]3[CH:36]=[C:7]([Br:18])[C:8](=[O:15])[CH:9]([CH3:14])[CH2:10][C:11]#[C:12][CH3:13])[CH2:29]2)[O:27]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 67184N-bromobutanimideHCID 110426053-Methyl-2-oxohept-5-ynylphosphonic acid dimethyl esterHCID 13245601(lR,5S,6R,7R)-3,3-ethylenedioxy-7-benzoyloxy-6formylbicyclo [3.3.0]octane

生成物 1

HCID 56607337
(1R,5S,6S,7R)-3,3-Ethylenedioxy-7-benzoyloxy-6-[(4RS)-2-bromo-4-methyl-3-oxooct-1-en-6-ynyl]bicyclo[3.3.0]octane

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒3 回

反応条件

温度
0 °C

実験手順

At 0° C., a solution of 10.5 g of 3-methyl-2-oxohept-5-ynephosphonic acid dimethyl ester in 70 ml of dimethoxyethane is added dropwise to a suspension of 1.81 g of sodium hydride in 180 ml of dimethoxyethane; the mixture is stirred for one hour at 0° C. and then 7.4 g of finely pulverized N-bromosuccinimide is added thereto. The mixture is agitated for 30 minutes at 0° C., combined with a solution of 11.4 g of (1R,5S,6R,7R)-3,3-ethylenedioxy-7-benzoyloxy-6-formylbicyclo[3.3.0]octane in 90 ml of dimethoxyethane, and agitated for 2 hours at 0° C. The reaction mixture is poured on saturated ammonium chloride solution and extracted with ether. The organic extract is washed neutral with water, dried over magnesium sulfate, and evaporated under vacuum. Chromatography of the residue on silica gel yields, with hexane/ether (3+2), 8.2 g of the unsaturated ketone as a colorless oil.

後処理

  1. stirringThe mixture is agitated for 30 minutes at 0° C.
  2. stirringagitated for 2 hours at 0° C
  3. extractionextracted with ether
  4. extractionThe organic extract
  5. washis washed neutral with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-449ee6b739044680a6baa7bc0ed95c3d
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05157042

反応ノート

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