1-(2-Methoxyphenyl)piperazine → 3-[4-[1-(2-Methoxyphenyl)-4-piperazinyl]butyl]-2-Methyl-4-thiazolidinone

HRID 846420ノート

反応式

HRID 846420 の反応式
[CH3:1][CH:2]1[N:6]([CH2:7][CH2:8][CH2:9][CH2:10]Br)[C:5](=[O:12])[CH2:4][S:3]1.[CH3:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>CC#N>[CH3:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[CH2:26][CH2:25][N:24]([CH2:10][CH2:9][CH2:8][CH2:7][N:6]2[C:5](=[O:12])[CH2:4][S:3][CH:2]2[CH3:1])[CH2:23][CH2:22]1

参加物

6

反応物 4

HCID 13461-(2-Methoxyphenyl)piperazineHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 104909933-(4-Bromobutyl)-2-methyl-4-thiazolidinone

生成物 1

HCID 156623253-[4-[1-(2-Methoxyphenyl)-4-piperazinyl]butyl]-2-Methyl-4-thiazolidinone

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A suspension of 2-methyl-3-(4-bromobutyl)-4-thiazolidinone (3.0 g), 1-(2-methoxyphenyl)piperazine (2.3 g), anhydrous K2CO3 (3.5 g) and NaI (200 mg) in 100 ml of anhydrous CH3CN was heated to 80° under N2. After 4 hours no starting material remained as judged by TLC. The mixture was cooled to room temperature, filtered and concentrated in vauco. The residue was chromatographed on silica, using EtOAc as the eluent. This provided 2.18 g of product as a clear oil which solidified in vacuo (0.1 mmHg) overnight.

後処理

  1. temperaturewas heated to 80° under N2
  2. filtrationfiltered
  3. concentrationconcentrated in vauco
  4. customThe residue was chromatographed on silica
  5. customsolidified in vacuo (0.1 mmHg) overnight

出典と根拠

ORDレコード
ord-7225c03122df48dc911763a8e27c0482
出典データセット
uspto-grants-1992_08
特許番号
US05136037

反応ノート

読み込み中…