Pyridine → HCID 20034593, 화합물

HRID 231123

반응식

HRID 231123 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 20034593HCID 20034593, 화합물수율 108.9%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매2회HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7865c18e0e4847a6b3d2252f1c412f04
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845113

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