ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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 2050558
ノート
印刷プレビュー

反応式

HRID 2050558 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 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. The mixture is stirred for 30 minutes at 0° C., combined with a solution of 11.4 g of (lR,5S,6R,7R)-3,3-ethylenedioxy-7-benzoyloxy-6formylbicyclo [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. After chromatographing the residue on silica gel, 8.2 g of the unsatura-ted ketone is obtained as a colorless oil with hexane/ether (3+2).

後処理

  1. stirringThe mixture is stirred 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-1b45ff08775c4f798271e392e859b17f
出典データセット
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05013758

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート