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

HRID 846420

반응식

HRID 846420 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7225c03122df48dc911763a8e27c0482
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05136037

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