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Hydrochloric Acid → HCID 87238501、化合物

HRID 442718
ノート
印刷プレビュー

反応式

HRID 442718 の反応式
C1([O:7]C)C=CC=CC=1.Cl.[OH-:10].[Na+].[C:12]([O:15]CC)(=[O:14])[CH3:13]>>[OH2:7].[C:12]([OH:15])(=[O:14])[C:13]([OH:7])=[O:10].[C:12]([OH:15])(=[O:14])[C:13]([OH:7])=[O:10]
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 4

HCID 313Hydrochloric AcidHCID 7519AnisoleHCID 8857Ethyl Acetate2 回HCID 14798Sodium Hydroxide

生成物 1

HCID 87238501HCID 87238501、化合物

実験手順

Under an inert atmosphere, 1.9 g of the previous compound are dissolved in 20 ml of anhydrous ethyl acetate and 5 ml of anisole and 20 ml of a 5N solution of HCl in ethyl acetate are added slowly at 5° C. The mixture is allowed to attain room temperature and after being stirred for 2 hours is cooled to about 5° C. before a 5N aqueous solution of NaOH is added to give a basic pH. The organic phase is then separated, dried and concentrated at about 70° C. under reduced pressure. The residual oil is dissolved in 60 ml of isopropanol and decolorized by means of 50 mg of active charcoal and 50 ml of a 0.5M solution of oxalic acid dihydrate in isopropanol are added; the precipitated salt is isolated by filtration. 1.5 g of oxalate hemihydrate are thus obtained (containing two molecules of oxalic acid), M.p.=130° C.

後処理

  1. customto attain room temperature
  2. additionis added
  3. customto give a basic pH
  4. customThe organic phase is then separated
  5. customdried
  6. concentrationconcentrated at about 70° C. under reduced pressure
  7. dissolutionThe residual oil is dissolved in 60 ml of isopropanol
  8. additionare added
  9. customthe precipitated salt is isolated by filtration

出典と根拠

ORDレコード
ord-9bcdffc113a9488fa561a44eb5a2768e
出典データセット
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05891893

反応ノート

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