Triethylamine → HCID 19989877、化合物

HRID 973424

反応式

HRID 973424 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.[N:19]1[CH:24]=[CH:23][CH:22]=[N:21][C:20]=1[N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.C(N(CC)CC)C>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:20]3[N:19]=[CH:24][CH:23]=[CH:22][N:21]=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

5

反応物 3

HCID 8471TriethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 199898454-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one

生成物 1

HCID 19989877HCID 19989877、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To 60 mL of toluene was added 4.0 g (0.0152 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.0 g (0.033 mol) of 1-(2-pyrimidyl)piperazine, and 4.0 g (0.04 mol) of triethylamine. The reaction mixture was heated at reflux for 2 days and subsequently washed with 2×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. Crystallization from ethyl acetate afforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 2 days
  3. washsubsequently washed with 2×50 mL of 1N NaOH
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customCrystallization from ethyl acetate
  8. customafforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.

出典と根拠

ORDレコード
ord-4468c9561fd34ace85f1afffbda719ff
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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