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Sodium Hydroxide → HCID 20568844, 화합물

HRID 1578097
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HRID 1578097 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)=O.[OH-:18].[Na+]>C(O)C>[CH3:4][C:5]1[N:1]=[C:2]2[CH:7]=[C:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:5]=[CH:4][N:3]2[C:8](=[O:18])[C:6]=1[CH2:7][CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 7015521Ethyl 2-aminopyridine-4-carboxylate

생성물 1

HCID 20568844HCID 20568844, 화합물수율 42%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.02 moles of 2-amino-4-ethoxycarbonylpyridine and 0.02 moles of ethyl-2-ethylacetacetate are stirred in a mixture of 10 ml. of phosphorous oxychloride and 2 g. of polyphosphoric acid at 120° C. for 2 hours. The reaction mixture is treated with 20 ml. of ethanol at 70° to 80° C., whereupon it is neutralized with a 10% (w/v) aqueous sodium hydroxide solution with ice cooling. The ethanol is evaporated, the residue is extracted with four 25-ml. portions of chloroform and the combined extracts are dried and evaporated. The evaporation residue is triturated with ether to give crystalline 2-methyl-3-ethyl-8-ethoxycarbonyl-4-oxo-4H-pyrido-(1,2-a)pyrimidine, melting at 95° to 96° C. Yield 42%. The product does not give any melting point depression when admixed with the product of Example 17.

후처리

  1. additionThe reaction mixture is treated with 20 ml
  2. customat 70° to 80° C.
  3. customThe ethanol is evaporated
  4. extractionthe residue is extracted with four 25-ml
  5. dry with materialportions of chloroform and the combined extracts are dried
  6. customevaporated
  7. customThe evaporation residue is triturated with ether

출처 및 근거

ORD 기록
ord-83a59a18e0a745b48b046a8007b2ac9d
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04291036

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