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1-(2-Methoxyphenyl)piperazine → HCID 21473675, 화합물

HRID 2294030
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HRID 2294030 반응식
Br.Br.Br[CH2:4][C:5]1[C:6]([NH2:14])=[N:7][C:8]([CH2:11][CH2:12][CH3:13])=[N:9][CH:10]=1.[CH3:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][N:26]([CH2:4][C:5]2[C:6]([NH2:14])=[N:7][C:8]([CH2:11][CH2:12][CH3:13])=[N:9][CH:10]=2)[CH2:25][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 11430Potassium CarbonateHCID 21473668HCID 21473668, 화합물

생성물 1

HCID 21473675HCID 21473675, 화합물수율 21%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 7.0 g (0.020 mol) of 5-bromomethyl-2-propyl-pyrimidin-4-ylamine dihydrobromide, 3.85 g (0.020 mol) of (2-methoxy-phenyl)-piperazine and 6 g (0.043 mol) of dry potassium carbonate in 75 ml of dimethylformamide was dissolved at room temperature for 4 hours. The reaction mixture was suction filtered, the filter cake was washed with ethyl acetate and ethanol, the filtrate was completely freed from the solvents and the residue was chromatographed over silica gel with ethyl acetate as the eluent and recrystallized from hot ethyl acetate. 1.3 g (21%) of 5-[4-(2-methoxy-phenyl)-piperazin-1-ylmethyl]-2-propyl-pyrimidin-4-ylamine were obtained as yellowish crystals, m.p. 130°.

후처리

  1. dissolutionwas dissolved at room temperature for 4 hours
  2. filtrationfiltered
  3. washthe filter cake was washed with ethyl acetate and ethanol
  4. customthe residue was chromatographed over silica gel with ethyl acetate as the eluent
  5. customrecrystallized from hot ethyl acetate

출처 및 근거

ORD 기록
ord-1cf885c9b94741c69ec69a32278410c1
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05688798

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