Potassium Carbonate → N,N-Diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine

HRID 437762

반응식

HRID 437762 반응식
ClC1C=C(C)N=C(C2C=CN=CC=2)N=1.Cl.C(NCC)C.C(=O)([O-])[O-].[K+].[K+].Cl.Cl.[CH2:29]([N:31]([CH2:45][CH3:46])[C:32]1[CH:37]=[C:36]([CH3:38])[N:35]=[C:34]([C:39]2[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=2)[N:33]=1)[CH3:30]>O.C(O)C>[CH2:45]([N:31]([CH2:29][CH3:30])[C:32]1[CH:37]=[C:36]([CH3:38])[N:35]=[C:34]([C:39]2[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=2)[N:33]=1)[CH3:46]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 10197650Diethylammonium chlorideHCID 127647054-Chloro-6-methyl-2-(pyridin-4-yl)pyrimidineHCID 12764719N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride

생성물 1

HCID 12764718N,N-Diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture containing 8.2 g. of 4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine, 8.7 g. of diethylamine hydrochloride, 100 ml. of ethanol, 6 g. of potassium carbonate and 10 ml. of water was refluxed with stirring for eight hours and then concentrated in vacuo to dryness. The residue was swirled in water and the solid collected. The solid was dissolved in boiling isopropyl alcohol, the hot solution treated with decolorizing charcoal and filtered, and the hot filtrate allowed to cool. The filtrate was then saturated with gaseous hydrogen chloride, ether was added to turbidity and the mixture was allowed to stand. The separated solid was collected and dried in vacuo at 80° C. to yield 7.4 g. of N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride, m.p. 205°-208° C.

후처리

  1. additionA mixture containing 8.2 g
  2. concentrationconcentrated in vacuo to dryness
  3. customthe solid collected
  4. dissolutionThe solid was dissolved
  5. additionthe hot solution treated with decolorizing charcoal
  6. filtrationfiltered
  7. temperatureto cool
  8. additionsaturated with gaseous hydrogen chloride, ether was added to turbidity
  9. customThe separated solid was collected
  10. customdried in vacuo at 80° C.
  11. customto yield 7.4 g

출처 및 근거

ORD 기록
ord-75972cc5fec742c895ee16a4f27e5f2d
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032523

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