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1-(2-Methoxyphenyl)piperazine → HCID 21473675、化合物

HRID 2294030
ノート
印刷プレビュー

反応式

HRID 2294030 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 11430Potassium CarbonateHCID 21473668HCID 21473668、化合物

生成物 1

HCID 21473675HCID 21473675、化合物収率 21%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-1cf885c9b94741c69ec69a32278410c1
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05688798

反応ノート

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