1-Phenylpiperazine → 3,4-Dihydro-2-methyl-4-[2-(4-phenyl-1-piperazinyl)ethyl]pyrimido[1,6-a]benzimidazol-1(2H)-one

HRID 973422

反応式

HRID 973422 の反応式
Cl[CH2:2][CH2:3][CH:4]1[C:9]2=[N:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:8]2[C:7](=[O:17])[N:6]([CH3:18])[CH2:5]1.[C:19]1([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C1(C)C=CC=CC=1>[CH3:18][N:6]1[CH2:5][CH:4]([CH2:3][CH2:2][N:28]2[CH2:29][CH2:30][N:25]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:26][CH2:27]2)[C:9]2=[N:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:8]2[C:7]1=[O:17]

参加物

4

反応物 2

HCID 70961-PhenylpiperazineHCID 199898454-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one

生成物 1

HCID 199898503,4-Dihydro-2-methyl-4-[2-(4-phenyl-1-piperazinyl)ethyl]pyrimido[1,6-a]benzimidazol-1(2H)-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To 4.0 g (0.015 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one in 35 mL of toluene was added 6.5 g (0.04 mol) of N-phenylpiperazine. The reaction mixture was heated to reflux for 2 days. The entire reaction mixture was washed with 3×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was subjected to preparative HPLC using acetone as the eluent and silica gel as the stationary phase. Like fractions were combined, concentrated and the residue crystallized from isopropyl alcohol to give 3.7 g (64%) of analytically pure, crystalline material, mp 143.5°-145.5° C.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 2 days
  3. customThe entire reaction mixture
  4. washwas washed with 3×50 mL of 1N NaOH
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated by rotary evaporation
  8. concentrationconcentrated
  9. customthe residue crystallized from isopropyl alcohol
  10. customto give 3.7 g (64%) of analytically pure, crystalline material, mp 143.5°-145.5° C.

出典と根拠

ORDレコード
ord-ada81d8a687f4554b66e8723a64677dc
出典データセット
uspto-grants-1991_11
特許番号
US05063228

関連ノート

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