Potassium Carbonate → 2-[{4-(1-Imidazolylmethyl)benzylideneamino}oxy]ethyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

HRID 1975603ノート

反応式

HRID 1975603 の反応式
[CH3:1][C:2]1[NH:3][C:4]([CH3:27])=[C:5]([C:23]([O:25][CH3:26])=[O:24])[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:7]=1[C:8]([O:10][CH2:11][CH2:12]Cl)=[O:9].[NH:28]1[CH:32]=[CH:31][N:30]=[C:29]1[CH2:33][C:34]1[CH:42]=[CH:41][C:37]([CH:38]=[N:39][OH:40])=[CH:36][CH:35]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:1][C:2]1[NH:3][C:4]([CH3:27])=[C:5]([C:23]([O:25][CH3:26])=[O:24])[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:7]=1[C:8]([O:10][CH2:11][CH2:12][O:40][N:39]=[CH:38][C:37]1[CH:36]=[CH:35][C:34]([CH2:33][C:29]2[NH:30][CH:31]=[CH:32][N:28]=2)=[CH:42][CH:41]=1)=[O:9]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 30168882-Chloroethyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylateHCID 867475924-(1-Imidazolylmethyl)benzaldoxime

生成物 1

HCID 867475912-[{4-(1-Imidazolylmethyl)benzylideneamino}oxy]ethyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

##STR36## 301 mg (0.763 mM) of 2-chloroethyl methyl 1,4-dihydro2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate and 155 mg (0.763 mM) of 4-(1-imidazolylmethyl)benzaldoxime were dissolved in 5 ml of dried acetonitrile, and then to the solution 58 mg (0.42 mM) of anhydrous potassium carbonate was added. After the mixture was heated under reflux for 15 hours, acetonitrile was distilled away and dichloromethane was added to the residue. After washing with water, the residue was dried over anhydrous sodium sulfate and dichloromethane was distilled away, and then the crystals were recrystallized from methanol, whereby the captioned compound was obtained. The yield was 400 mg (94%).

後処理

  1. temperatureAfter the mixture was heated
  2. temperatureunder reflux for 15 hours
  3. distillationacetonitrile was distilled away
  4. additiondichloromethane was added to the residue
  5. washAfter washing with water
  6. dry with materialthe residue was dried over anhydrous sodium sulfate and dichloromethane
  7. distillationwas distilled away
  8. customthe crystals were recrystallized from methanol, whereby the captioned compound
  9. customwas obtained

出典と根拠

ORDレコード
ord-e7e4464e74fa4aa0ba877773174fb7e0
出典データセット
uspto-grants-1994_02
特許番号
US05286869

反応ノート

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