Phenethylamine → 1-(6-Phenethylamino-pyrimidin-4-yl)-8-phenyl-1,2,3,4-tetrahydro-pyrido[1,2-a]pyrimidin-6-one

HRID 1785471노트

반응식

HRID 1785471 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][CH2:11][N:10]3[C:14](=[O:24])[CH:15]=[C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH:17]=[C:9]23)[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH2:31]([NH2:39])[CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>CN(C=O)C.O.CCOC(C)=O>[CH2:31]([NH:39][C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][CH2:11][N:10]3[C:14](=[O:24])[CH:15]=[C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH:17]=[C:9]23)[CH:3]=1)[CH2:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1

참가 물질

7

반응물 3

HCID 1001PhenethylamineHCID 11430Potassium CarbonateHCID 575931531-(6-Chloro-pyrimidin-4-yl)-8-phenyl-1,2,3,4-tetrahydro-pyrido[1,2-a]pyrimidin-6-one

생성물 1

HCID 114301641-(6-Phenethylamino-pyrimidin-4-yl)-8-phenyl-1,2,3,4-tetrahydro-pyrido[1,2-a]pyrimidin-6-one

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirred mixture of 1-(6-chloro-pyrimidin-4-yl)-8-phenyl -1,2,3,4-tetrahydro-pyrido[1,2-a]pyrimidin-6-one (0.158 mg, 0.47 mmol) and excess of K2CO3 in DMF (3 mL) was added phenethylamine (0.15 mL, 1.2 mmol). The overall reaction vessel was irradiated under microwave conditions at 150° C. for 10 min. After diluted with water and EtOAc, the organic layer was taken and the aqueous layer was extracted with EtOAc. The overall organic layers were washed with water, brine, and dried (Na2SO4). Filtration followed by evaporation gave the crude residue, which was washed with EtOAc/ether to provide the title compound as a light yellow solid. MS m/e 424 (M+H)+.

후처리

  1. customThe overall reaction vessel was irradiated under microwave conditions at 150° C. for 10 min
  2. extractionthe aqueous layer was extracted with EtOAc
  3. washThe overall organic layers were washed with water, brine
  4. dry with materialdried (Na2SO4)
  5. filtrationFiltration
  6. customfollowed by evaporation
  7. customgave the crude residue, which
  8. washwas washed with EtOAc/ether

출처 및 근거

ORD 기록
ord-b2f3937799494752b8fbf7e0af1f7829
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504403B2

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