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Potassium Carbonate → HCID 57565950、化合物

HRID 1728167
ノート
印刷プレビュー

反応式

HRID 1728167 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].Br[CH2:12][CH2:13][O:14][C:15](=[O:17])[CH3:16].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:10][CH2:12][CH2:13][O:14][C:15](=[O:17])[CH3:16])=[C:6]([CH:7]=[O:8])[CH:9]=1
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 11430Potassium CarbonateHCID 124815-Chloro-salicylaldehydeHCID 135641-Acetoxy-2-bromoethane

生成物 1

HCID 57565950HCID 57565950、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5-Chloro-2-hydroxy-benzaldehyde (2 g, 12.8 mmol), acetic acid 2-bromo-ethyl ester (2.57 g, 15.4 mmol), K2CO3 (5.3 g, 38.5 mmol) and KI (0.26 g, 1.54 mmol) were mixed in DMF (20 mL). Then the reaction tube was placed into the cavity of a focused monomode microwave reactor and the contents of the flask were irradiated at 130° C. for 30 min. The mixture was filtered and the filtrate was concentrated. The residue was dissolved in CH2Cl2 and the organic layer was washed with water for several times. Then the organic layer was dried over anhydrous Na2SO4 and concentrated to obtain a yellow solid. (2.7 g)

後処理

  1. customThen the reaction tube was placed into the cavity of a focused monomode microwave reactor
  2. customthe contents of the flask were irradiated at 130° C. for 30 min
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved in CH2Cl2
  6. washthe organic layer was washed with water for several times
  7. dry with materialThen the organic layer was dried over anhydrous Na2SO4
  8. concentrationconcentrated
  9. customto obtain a yellow solid

出典と根拠

ORDレコード
ord-91dab68b39774aecadcbe31ac2cca493
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07495007B2

反応ノート

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