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1-Methylpiperazine → 3-[4-(4-Chlorophenyl)-2-(4-methyl-1-piperazinyl)-5-oxazolyl]propionic acid

HRID 350728
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인쇄 미리보기

반응식

HRID 350728 반응식
Cl[C:2]1[O:3][C:4]([CH2:14][CH2:15][C:16]([OH:18])=[O:17])=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[N:6]=1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(O)(C)C>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]([C:5]2[N:6]=[C:2]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[O:3][C:4]=2[CH2:14][CH2:15][C:16]([OH:18])=[O:17])=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 118082582-Chloro-4-(4-chlorophenyl)-5-oxazolepropionic acid

생성물 1

HCID 210886393-[4-(4-Chlorophenyl)-2-(4-methyl-1-piperazinyl)-5-oxazolyl]propionic acid수율 78.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixed solution of 3-[2-chloro-4-(4-chlorophenyl)-5-oxazolyl]propionic acid (1.43 g), 1-methylpiperazine (2.5 g) and isopropyl alcohol (20 mL) was heated under reflux for 10 hrs. The reaction mixture was concentrated, diluted with water, and acidified with 2N aqueous hydrochloric acid solution. The precipitated crystals were collected by filtration and recrystallized from ethanol to give 3-[4-(4-chlorophenyl)-2-(4-methyl-1-piperazinyl)-5-oxazolyl]propionic acid (1.37 g, yield 70%) as colorless prism crystals. melting point: 157–160° C.

후처리

  1. temperatureunder reflux for 10 hrs
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with water
  4. filtrationThe precipitated crystals were collected by filtration
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-2b259809568d4908875b16275f2ff930
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07183276B2

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