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

HRID 973423

반응식

HRID 973423 반응식
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]=[CH: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[CH:21]=[CH:22][CH:23]=[CH:24][N:19]=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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 944591-(2-Pyridyl)piperazineHCID 199898454-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one

생성물 1

HCID 199898433,4-Dihydro-2-methyl-4-[2-[4-(2-pyridinyl)-1-piperazinyl]ethyl]-pyrimido[1,6-a]benzimidazol-1(2H)-one

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To 50 mL of toluene was added 5.0 g (0.019 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.19 g (0.038 mol) of 1-(2-pyridyl)piperazine, and 3.8 g (0.038 mol) of triethylamine. The reaction mixture was heated to reflux for 24 hours. The reaction mixture was washed with 2×50 mL of NaOH, dried over Na2SO4, filtered and concentrated by rotary evaporation. The residue was crystallized from isopropyl alcohol to afford 5.5 g (75%) of analytically pure crystals, mp 158°-59° C.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. washThe reaction mixture was washed with 2×50 mL of NaOH
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customThe residue was crystallized from isopropyl alcohol
  8. customto afford 5.5 g (75%) of analytically pure crystals, mp 158°-59° C.

출처 및 근거

ORD 기록
ord-ad422870f78846f689801171972dfbb1
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05063228

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