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

HRID 64591노트

반응식

HRID 64591 반응식
[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]

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-67302bf687d1411993f63793eafa3376
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609494

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