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

HRID 1785471ノート

反応式

HRID 1785471 の反応式
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

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-b2f3937799494752b8fbf7e0af1f7829
出典データセット
uspto-grants-2009_03
特許番号
US07504403B2

反応ノート

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