Potassium Carbonate → Methyl 3-(2-(cyclohexylamino)-2-oxoethyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate

HRID 1094707ノート

反応式

HRID 1094707 の反応式
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][CH:7]=[N:6][C:5]=2[S:4][C:3]=1[C:12]([O:14][CH3:15])=[O:13].C([O-])([O-])=O.[K+].[K+].Cl[CH2:23][C:24]([NH:26][CH:27]1[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1)=[O:25]>CC#N>[CH:27]1([NH:26][C:24](=[O:25])[CH2:23][N:8]2[C:9](=[O:11])[C:10]3[C:2]([CH3:1])=[C:3]([C:12]([O:14][CH3:15])=[O:13])[S:4][C:5]=3[N:6]=[CH:7]2)[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2223652-Chloro-N-cyclohexylacetamideHCID 725279Methyl 5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate

生成物 1

HCID 1093519Methyl 3-(2-(cyclohexylamino)-2-oxoethyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of methyl 5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate (2.24 g, 10 mmol) in CH3CN (25 mL) was added K2CO3 (1.38 g, 10 mmol), KI (1.61 g, 10 mmol), and 2-chloro-N-cyclohexylacetamide (1.75 g, 10 mmol). The reaction mixture was refluxed overnight and quenched with H2O (120 mL). The resulting precipitate was filtered and dried to afford methyl 3-(2-(cyclohexylamino)-2-oxoethyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate, as a solid (yield: quantitative).

後処理

  1. temperatureThe reaction mixture was refluxed overnight
  2. customquenched with H2O (120 mL)
  3. filtrationThe resulting precipitate was filtered
  4. customdried

出典と根拠

ORDレコード
ord-f5187db793014a8b862031953592493d
出典データセット
uspto-grants-2012_03
特許番号
US08133998B2

反応ノート

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