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p-Toluenesulfonic acid → 9-Methyl-2-propyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1580941
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인쇄 미리보기

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HRID 1580941 반응식
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9]([CH2:14][C:15](OC)=[O:16])(=O)[CH2:10][CH2:11][CH3:12].C1(C)C=CC(S(O)(=O)=O)=CC=1>COCCO>[CH3:8][C:7]1[C:2]2=[N:1][C:9]([CH2:10][CH2:11][CH3:12])=[CH:14][C:15](=[O:16])[N:3]2[CH:4]=[CH:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 153472-Amino-3-methylpyridineHCID 121700Methyl 3-oxohexanoate

생성물 1

HCID 123397189-Methyl-2-propyl-4H-pyrido[1,2-a]pyrimidin-4-one

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

반응 조건

온도
-30 °C

실험 절차

A solution of 54.0g of 2-amino-3-methylpyridine, 144.0g of methyl butyrylacetate, 5.0g of p-toluenesulfonic acid, and 750ml of ethylene glycol monomethyl ether is heated in a nitrogen atmosphere, under reflux, for 60 hours. The solution is concentrated to dryness in vacuo, and the residual oil extracted with two 250ml portions of pentane. The pentane solution is concentrated to a volume of 250ml and cooled at -30°C to yield the title compound, melting point 59°-60°C.

후처리

  1. temperatureunder reflux, for 60 hours
  2. concentrationThe solution is concentrated to dryness in vacuo
  3. extractionthe residual oil extracted with two 250ml portions of pentane
  4. concentrationThe pentane solution is concentrated to a volume of 250ml

출처 및 근거

ORD 기록
ord-2ee1cbf26f2e46e4a3dca42e0247362c
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03935197

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