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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
ノート
印刷プレビュー

反応式

HRID 1788751 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4b02aacf4a8944cd8a856d38eed02d31
出典データセット
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04684655

反応ノート

読み込み中…

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