Pyridine → HCID 20034593、化合物

HRID 231123

反応式

HRID 231123 の反応式
[C:1]1([CH:7]2[CH2:9][CH:8]2[C:10](Cl)=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:13][C:14]1(C)[O:19]C(=O)[CH2:17][C:16](=O)[O:15]1.N1C=CC=CC=1.OS(O)(=O)=O>ClCCCl.O>[C:1]1([CH:7]2[CH2:9][CH:8]2[C:10](=[O:11])[CH2:13][C:14]([O:15][CH2:16][CH3:17])=[O:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 1049PyridineHCID 1118Sulfuric AcidHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 523092Cyclopropanecarbonyl chloride, 2-phenyl-

生成物 1

HCID 20034593HCID 20034593、化合物収率 108.9%

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒2 回HCID 962Water溶媒

実験手順

A solution of 2-phenyl-1-cyclopropanecarboxylic acid chloride (15 g) in 1,2-dichloroethane (70 ml) is added at 0° C. to a solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (Meldrum's acid, 12 g) and pyridine (13.2 g) in 1,2-dichloroethane (70 ml) and the solution is stirred at room temperature for one hour. A 2N water solution of H2SO4 (20 ml) is then added, the two layers are separated and the organic phase is washed twice with water (50 ml), dryed on Na2SO4 and evaporated in vacuum. The residue is dissolved in EtOH (150 ml), heated to the reflux temperature for two hours and evaporated to dryness to give almost pure ethyl 3-(2-phenyl-1-cyclopropyl)-3-oxo-propanoate (21 g).

後処理

  1. customthe two layers are separated
  2. washthe organic phase is washed twice with water (50 ml)
  3. customevaporated in vacuum
  4. dissolutionThe residue is dissolved in EtOH (150 ml)
  5. temperatureheated to the reflux temperature for two hours
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-7865c18e0e4847a6b3d2252f1c412f04
出典データセット
uspto-grants-1989_07
特許番号
US04845113

関連ノート

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