Potassium Carbonate → Ethyl 3-acetyl-1,2,3,4-tetrahydro-4-(2-hydroxy-5-nitrophenyl)-6-methyl-2-oxo-5-pyrimidinecarboxylate

HRID 64591ノート

反応式

HRID 64591 の反応式
[C:1]([N:4]1[CH:9]([C:10]2[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:11]=2[O:19]C(=O)C)[C:8]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[C:7]([CH3:28])[NH:6][C:5]1=[O:29])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl-].[NH4+]>C(O)C>[C:1]([N:4]1[CH:9]([C:10]2[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:11]=2[OH:19])[C:8]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[C:7]([CH3:28])[NH:6][C:5]1=[O:29])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 20236390Ethyl 3-acetyl-1,2,3,4-tetrahydro-4-(2-acetoxy-5-nitrophenyl)-6-methyl-2-oxo-5-pyrimidine carboxylate

生成物 1

HCID 20236388Ethyl 3-acetyl-1,2,3,4-tetrahydro-4-(2-hydroxy-5-nitrophenyl)-6-methyl-2-oxo-5-pyrimidinecarboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of the Compound 1a (1.03 g) in ethanol (60 mL) at ambient temperature was added potassium carbonate (2.0 g). After stirring for 18 hours, to the reaction mixture was added saturated aqueous ammonium chloride. The reaction mixture was then extracted with methylene chloride and the combined organic extracts were dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue purified by flash chromatography on silica gel eluted with methanol:methylene chloride (3:97) to yield the desired product as a solid.

後処理

  1. extractionThe reaction mixture was then extracted with methylene chloride
  2. dry with materialthe combined organic extracts were dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo
  5. customthe residue purified by flash chromatography on silica gel
  6. washeluted with methanol:methylene chloride (3:97)

出典と根拠

ORDレコード
ord-67302bf687d1411993f63793eafa3376
出典データセット
uspto-grants-1986_09
特許番号
US04609494

反応ノート

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