Sodium Iodide → Ethyl 2-acetyl-4-[4-(4-fluorobenzoyl)piperidino]-butyrate

HRID 1461739

반응식

HRID 1461739 반응식
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[H-].[Na+].[I-].[Na+].Cl[CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][CH:20]([C:23](=[O:31])[C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[CH2:19][CH2:18]1>O1CCCC1>[C:3]([CH:2]([CH2:15][CH2:16][N:17]1[CH2:18][CH2:19][CH:20]([C:23](=[O:31])[C:24]2[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=2)[CH2:21][CH2:22]1)[C:1]([O:7][CH2:8][CH3:9])=[O:6])(=[O:4])[CH3:5]

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 8868Ethyl AcetoacetateHCID 24758Sodium hydrideHCID 10516150Methanone, [1-(2-chloroethyl)-4-piperidinyl](4-fluorophenyl)-

생성물 1

HCID 14882705Ethyl 2-acetyl-4-[4-(4-fluorobenzoyl)piperidino]-butyrate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
20 °C

실험 절차

A solution of 5.45 g of ethyl acetoacetate in 20 ml of tetrahydrofuran is added at 0° C. to a suspension of 1.68 g of sodium hydride at a concentration of 60% in oil in 100 ml of anhydrous tetrahydrofuran. The medium is maintained at 20° C. for 1 hour 30 minutes. 6.3 g of sodium iodide are added, followed by the addition at 0° C. of 11.3 g of 1-(2-chloroethyl)-4-(4-fluorobenzoyl)piperidine in 100 ml of tetrahydrofuran. The reaction mixture is brought to reflux for 15 hours. It is concentrated under vacuum. The residue is taken up in water and the product is extracted with dichloromethane.

후처리

  1. temperatureto reflux for 15 hours
  2. concentrationIt is concentrated under vacuum
  3. extractionthe product is extracted with dichloromethane

출처 및 근거

ORD 기록
ord-eb99b06868674e2c9d29b38620f253b3
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05077288

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