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Benzene → HCID 57725029、化合物

HRID 1987778
ノート
印刷プレビュー

反応式

HRID 1987778 の反応式
[N+:1]([C:4]1[C:5]([CH3:21])=[C:6]2[C:11](=[C:12]([CH3:15])[C:13]=1[CH3:14])[O:10][C:9]([CH2:17][O:18][CH3:19])([CH3:16])[CH2:8][CH:7]2O)([O-:3])=[O:2].C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[N+:1]([C:4]1[C:5]([CH3:21])=[C:6]2[C:11](=[C:12]([CH3:15])[C:13]=1[CH3:14])[O:10][C:9]([CH2:17][O:18][CH3:19])([CH3:16])[CH:8]=[CH:7]2)([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 23118277HCID 23118277、化合物

生成物 1

HCID 57725029HCID 57725029、化合物収率 99.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 10.1 g of 6-nitro-4-hydroxy-2-methoxymethyl-2,5,7,8-tetramethylchroman, 200 ml of benzene was added and 1.0 g of p-toluenesulfonic acid was added, followed by heating at reflux for 2 hours using a Dean-Stark apparatus. The reaction solution was poured into water and then extracted with ethyl acetate. The organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution, washed with saturated saline and then dried over anhydrous magnesium sulfate. After removing magnesium sulfate by filtration and concentrating under reduced pressure, 9.4 g of the objective oily compound was obtained.

後処理

  1. temperatureby heating
  2. temperatureat reflux for 2 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution
  5. washwashed with saturated saline
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customAfter removing magnesium sulfate
  8. filtrationby filtration
  9. concentrationconcentrating under reduced pressure

出典と根拠

ORDレコード
ord-70ea1098134b4da5803b1fad1eec62f6
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07553837B2

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