Sodium hydride → HCID 54295833, 화합물

HRID 2225810노트

반응식

HRID 2225810 반응식
[CH2:1]([O:3][C:4](=[O:14])[C:5](=[O:13])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[CH3:2].[H-].[Na+].Br[CH2:18][C:19]([N:21]1[CH2:26][CH2:25][N:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:23][CH2:22]1)=[O:20]>CN(C)C=O>[CH2:1]([O:3][C:4](=[O:14])[C:5](=[O:13])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:18][C:19](=[O:20])[N:21]2[CH2:26][CH2:25][N:24]([C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)[CH2:23][CH2:22]2)=[CH:8][CH:7]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 11715332Ethyl 2-(4-hydroxyphenyl)-2-oxoacetateHCID 138085392-Bromo-1-(4-phenylpiperazin-1-yl)ethan-1-one

생성물 1

HCID 54295833HCID 54295833, 화합물수율 67.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of 4-hydroxy-alpha-oxobenzeneacetic acid ethyl ester (0.582 g) in dimethylformamide (8 mL) under argon was treated with 55% sodium hydride (0.131 g), stirred for 30 minutes in a ice-water bath and then 1-(bromoacetyl)-4-phenyl-piperazine (1.0 g) in dimethylformamide (5 mL) was added. The solution was stirred at room temperature for 18 hours and worked up as in Example 20. The crude product was purified by HPLC (ethyl acetate-hexane; 1:1) to yield 0.8 g of 4-[2-oxo-2-(4-phenyl-1-piperazinyl)ethoxy]-alpha-oxobenzeneacetic acid ethyl ester as an oil.

후처리

  1. stirringThe solution was stirred at room temperature for 18 hours
  2. customThe crude product was purified by HPLC (ethyl acetate-hexane; 1:1)

출처 및 근거

ORD 기록
ord-700a45020bca4d8c8c56b8094bda236e
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

반응 노트

불러오는 중…