1-(2-Hydroxyethyl)piperazine → 5-[3-(4-Methoxyphenyl)propyl]-5-[4-(2-hydroxyethyl)piperazinyl]barbituric Acid

HRID 993054ノート

反応式

HRID 993054 の反応式
Br[C:2]1([CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[C:7](=[O:8])[NH:6][C:5](=[O:9])[NH:4][C:3]1=[O:10].[OH:22][CH2:23][CH2:24][N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1>C(O)C>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([CH2:13][CH2:12][CH2:11][C:2]2([N:28]3[CH2:29][CH2:30][N:25]([CH2:24][CH2:23][OH:22])[CH2:26][CH2:27]3)[C:7](=[O:8])[NH:6][C:5](=[O:9])[NH:4][C:3]2=[O:10])=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 184086795-Bromo-5-[3-(4-methoxyphenyl)propyl]barbituric acid

生成物 1

HCID 184086745-[3-(4-Methoxyphenyl)propyl]-5-[4-(2-hydroxyethyl)piperazinyl]barbituric Acid収率 3.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A of 5-Bromo-5-[3-(4-Methoxyphenyl)propyl]barbituric Acid (710 mg) and N-(2-hydroxyethyl)piperazine (281 mg) in 25 ml of ethanol is refluxed for 4 hours. The solvent is evaporated under reduced pressure and the residue is partitioned between 1 N hydrochloric acid and ethyl acetate. The aqueous phase is basified to pH=6-7 and extracted with ethyl acetate. The organic phase is concentrated to dryness and the residue is crystallized from ethyl acetate to give 30 mg of the product.

後処理

  1. customThe solvent is evaporated under reduced pressure
  2. customthe residue is partitioned between 1 N hydrochloric acid and ethyl acetate
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic phase is concentrated to dryness
  5. customthe residue is crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-06b3964bb09e48b6a4ec998ca2b1d46c
出典データセット
uspto-grants-2002_10
特許番号
US06472396B1

反応ノート

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