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Hydrochloric Acid → 1,2,3,4-Tetrahydro-6-methyl-4-(3-nitrophenyl)-2-oxo-3-(3-phenylpropyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester

HRID 1788751
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HRID 1788751 반응식
C[O:2][C:3]1[N:4](CCCC2C=CC=CC=2)[CH:5]([CH3:24])[C:6]([C:18]([O:20][CH:21]([CH3:23])[CH3:22])=[O:19])=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[N:8]=1.Cl>CO>[CH3:24][C:5]1[NH:4][C:3](=[O:2])[N:8]([CH2:5][CH2:6][CH2:7][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[C:6]=1[C:18]([O:20][CH:21]([CH3:23])[CH3:22])=[O:19]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 572168171,6-Dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-1-(3-phenylpropyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester

생성물 1

HCID 138858631,2,3,4-Tetrahydro-6-methyl-4-(3-nitrophenyl)-2-oxo-3-(3-phenylpropyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester수율 169.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1,6-dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-1-(3-phenylpropyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester (1.96 g. 4.34 mmoles) in methanol (20 ml) was treated with 2.5 N hydrochloric acid (5 ml) and the resulting mixture was allowed to stir at room temperature overnight. A colorless solid precipitated out. Methanol was evaporated and the residue was taken up in ethyl acetate. The solution was washed with water, sodium bicarbonate solution and brine. It was dried over anhydrous magnesium sulfate and evaporated. The residue was crystallized from dichloromethane/isopropyl ether to provide the title compound as a colorless solid (1.61 g), melting point 149.5-151.5° C.

후처리

  1. customA colorless solid precipitated out
  2. customMethanol was evaporated
  3. washThe solution was washed with water, sodium bicarbonate solution and brine
  4. dry with materialIt was dried over anhydrous magnesium sulfate
  5. customevaporated
  6. customThe residue was crystallized from dichloromethane/isopropyl ether

출처 및 근거

ORD 기록
ord-4b02aacf4a8944cd8a856d38eed02d31
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04684655

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