Formaldehyde → 1-(4-Chlorophenyl)-3-(4-(2-methoxyethyl)piperazin-1-yl)methyl-2-pyrrolidinone

HRID 1533424ノート

反応式

HRID 1533424 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:12][CH2:11][CH:10]([C:13](O)=O)[C:9]2=[O:16])=[CH:4][CH:3]=1.[CH3:17][O:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C=O>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:12][CH2:11][CH:10]([CH2:13][N:24]3[CH2:25][CH2:26][N:21]([CH2:20][CH2:19][O:18][CH3:17])[CH2:22][CH2:23]3)[C:9]2=[O:16])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 712FormaldehydeHCID 27346381-(2-Methoxyethyl)piperazineHCID 40570841-(4-Chlorophenyl)-2-oxopyrrolidine-3-carboxylic acid

生成物 1

HCID 49132091-(4-Chlorophenyl)-3-(4-(2-methoxyethyl)piperazin-1-yl)methyl-2-pyrrolidinone収率 77.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

3.0 g of 1-(4-chlorophenyl)-3-carboxy-2-pyrrolidinone and 2.32 g of 4-(2-methoxyethyl)piperazine were mixed with 6 ml of methanol. Thereto was added 0.465 g of 80% paraformaldehyde. The mixture was subjected to a reaction for 10.5 hours under refluxing and then cooled to room temperature. Thereto was added 10 ml of methanol, and the insolubles were removed by filtration. The filtrate was concentrated under reduced pressure. The residue was mixed with 15 ml of water. The resulting crystals were collected by filtration and washed with 3 ml of 95% aqueous methanol twice to obtain 3.42 g of 1-(4-chlorophenyl)-3-[4-(2-methoxyethyl)piperazine-1-yl]methyl-2-pyrrolidinone.

後処理

  1. customThe mixture was subjected to a reaction for 10.5 hours
  2. temperatureunder refluxing
  3. customthe insolubles were removed by filtration
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. additionThe residue was mixed with 15 ml of water
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed with 3 ml of 95% aqueous methanol twice

出典と根拠

ORDレコード
ord-51dd2763b9d14ed19182712d95cc59b5
出典データセット
uspto-grants-2001_03
特許番号
US06207825B1

反応ノート

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