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Hydrochloric Acid → HCID 70631399, 화합물

HRID 372590
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HRID 372590 반응식
[NH2:1][C:2]1[C:9]([Br:10])=[CH:8][C:7]([Br:11])=[CH:6][C:3]=1[CH2:4]O.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C(O)(=O)CC.[ClH:24]>C(OCC)(=O)C>[ClH:24].[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([CH2:4][C:3]2[CH:6]=[C:7]([Br:11])[CH:8]=[C:9]([Br:10])[C:2]=2[NH2:1])[CH2:15][CH2:14]1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1032Propionic AcidHCID 531671-MethylpiperazineHCID 213204952-Amino-3,5-dibromobenzenemethanol

생성물 1

HCID 70631399HCID 70631399, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

A mixture of 0.56 part of 2-amino-3,5-dibromobenzylalcohol, 1.0 part of N-methyl piperazine and 2 parts of propionic acid is heated at 140° C for 8 hours under stirring. Then, the propionic acid is distilled off under reduced pressure. The residue is extracted with chloroform. The chloroform layer is washed with water and dried over sodium sulfate. Evaporation of the solvent gives oily residue. The residue is chromotographed over silica gel. Ethyl acetate eluates are treated with ethanolic hydrochloric acid. This procedure gives N1 -methyl-N4 -(2-amino-3,5-dibromobenzyl)piperazine hydrochloride melting at 182° to 185° C.

후처리

  1. distillationThen, the propionic acid is distilled off under reduced pressure
  2. extractionThe residue is extracted with chloroform
  3. washThe chloroform layer is washed with water
  4. dry with materialdried over sodium sulfate
  5. customEvaporation of the solvent
  6. customgives oily residue

출처 및 근거

ORD 기록
ord-d02da9a45bf74325877917a292ba46f6
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04091220

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