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Hydrochloric Acid → HCID 17816516、化合物

HRID 2249687
ノート
印刷プレビュー

反応式

HRID 2249687 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1O)[CH:5]=[O:6].[C:11](=[O:14])([O-])[O-].[K+].[K+].[CH2:17](I)[CH2:18][CH:19]([CH3:21])[CH3:20].Cl>CN(C)C=O.O.C(OCC)(=O)C>[CH2:17]([O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[O:14][CH2:11][CH2:3][CH:4]([CH3:7])[CH3:5])[CH:5]=[O:6])[CH2:18][CH:19]([CH3:21])[CH3:20]
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

8

反応物 4

HCID 313Hydrochloric AcidHCID 87683,4-DihydroxybenzaldehydeHCID 109241-Iodo-3-methylbutaneHCID 11430Potassium Carbonate

生成物 1

HCID 17816516HCID 17816516、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

In 50 ml of N,N-dimethylformamide are suspended 5.0 g of 3,4-dihydroxybenzaldehyde, 15.5 g of potassium carbonate and 14 ml of isopentyl iodide. The mixture is stirred at 60° C. for 2 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 6 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=10:1) to obtain 9.4 g of 3,4-diisopentyloxybenzaldehyde as a light yellow oily product.

後処理

  1. customthe organic layer is separated
  2. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride successively
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent is distilled off under reduced pressure
  5. customThe residue thus obtained
  6. customis purified by silica gel column chromatography (eluent; hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-b7ec15e2e8ea44d9b315a313ee4de17c
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

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