Potassium Carbonate → HCID 69529373、化合物

HRID 1634895ノート

反応式

HRID 1634895 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13]2[CH:18]=[C:17]([CH:19]=O)[CH:16]=[CH:15][N:14]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].C(OP([CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])(OCC)=O)C.C(=O)([O-])[O-].[K+].[K+]>C(O)(C)(C)C>[CH3:12][O:11][C:7]1[CH:6]=[C:5]([C:13]2[CH:18]=[C:17]([CH:19]=[CH:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])[CH:16]=[CH:15][N:14]=2)[CH:4]=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 13345Triethyl phosphonoacetateHCID 186750102-(3,4,5-Trimethoxyphenyl)pyridine-4-carboaldehyde

生成物 1

HCID 69529373HCID 69529373、化合物

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

2-(3,4,5-Trimethoxyphenyl)pyridine-4-carboaldehyde (507 mg) and ethyl diethylphosphonoacetate (570 μL) were dissolved in tert-butanol (16 mL), and to the solution potassium carbonate (438 mg) was added. The mixture was stirred for 3 hours under reflux and concentrated under reduced pressure. The residue was dissolved in chloroform, and the solution was washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to obtain the title compound.

後処理

  1. temperatureunder reflux
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in chloroform
  4. washthe solution was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-c634ae911fff4c32b5ded475a6b1c7d9
出典データセット
uspto-grants-2003_01
特許番号
US06509329B1

反応ノート

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