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Acetone → 2,6-Dichlorobenzylideneacetone

HRID 1807409
ノート
印刷プレビュー

反応式

HRID 1807409 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:3]=1[CH:4]=O.[CH3:11][C:12]([CH3:14])=[O:13].[OH-].[Na+]>O>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:3]=1/[CH:4]=[CH:11]/[C:12](=[O:13])[CH3:14]
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

5

反応物 3

HCID 180AcetoneHCID 67372,6-DichlorobenzaldehydeHCID 14798Sodium Hydroxide

生成物 1

HCID 57087852,6-Dichlorobenzylideneacetone収率 97.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

A round bottom flask equipped with magnetic stirrer and nitrogen inlet was charged with 2,6-dichlorobenzaldehyde (5.0 g, 28.57 mmol), acetone (42 ml, 0.571 mol) and water (20 ml). The mixture was cooled to 0° C. and a solution of sodium hydroxide (1.14 g, 28.57 mmol) in water (20 ml) was added drop wise during 1 hour to the vigorous stirred suspension. The reaction mixture was stirred for an additional 0.5 hour. The reaction mixture was concentrated in vacuo, poured onto 10% HCl (100 ml) and extracted with ethyl acetate (3×50 ml). Combined organic layers were dried over anhydrous sodium sulfate. The solvent was removed in vacuo and the residue was purified by flash chromatography over silica gel (350 g) (eluent: n-hexane/ethyl acetate 10:1) to afford 6.0 g (97% of theory) of (E)-4-(2,6-dichloro-phenyl)-but-3-en-2-one in form of a pale yellow oil.

後処理

  1. customA round bottom flask equipped with magnetic stirrer and nitrogen inlet
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additionpoured onto 10% HCl (100 ml)
  4. extractionextracted with ethyl acetate (3×50 ml)
  5. dry with materialCombined organic layers were dried over anhydrous sodium sulfate
  6. customThe solvent was removed in vacuo
  7. customthe residue was purified by flash chromatography over silica gel (350 g) (eluent: n-hexane/ethyl acetate 10:1)

出典と根拠

ORDレコード
ord-9d3b6ac7b2d64fa6a302af5a7cf639ef
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08357635B2

反応ノート

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