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Water → HCID 54547942, 화합물

HRID 582320
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HRID 582320 반응식
CO[C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18]3[C:23]([NH:24][CH:25]([CH3:27])[CH3:26])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:14][CH2:13]2)=[O:11])=[CH:6][CH:5]=1.[NH2:29][CH2:30][CH2:31][N:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1.O>C(O)C.C(#N)C>[CH:25]([NH:24][C:23]1[C:18]([N:15]2[CH2:16][CH2:17][N:12]([C:10]([C:7]3[CH:8]=[CH:9][C:4]([C:3](=[O:28])[NH:29][CH2:30][CH2:31][N:32]4[CH2:37][CH2:36][O:35][CH2:34][CH2:33]4)=[CH:5][CH:6]=3)=[O:11])[CH2:13][CH2:14]2)=[N:19][CH:20]=[CH:21][CH:22]=1)([CH3:27])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 4082852-MorpholinoethylamineHCID 537116704-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid methyl ester

생성물 1

HCID 54547942HCID 54547942, 화합물수율 81%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6342
Acetonitrile
용매

실험 절차

4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid methyl ester (1.2 g) was dissolved in a co-solvent of ethanol (10 ml) and acetonitrile (20 ml), and 4-(2-aminoethyl)morpholine (0.82 g) was added. The reaction mixture was heated to reflux for 15 hours and cooled. After excess of water was added to the solution at 30° C. to precipitate the crystals, the solution was stirred for 1 hour. Then, the solution was again cooled slowly, stirred at 10~15° C. for 2 hours and filtered. The filtered crystal was washed with preheated water(40° C.) and was recrystallized using isopropanol and ether, filtered and dried to give 1.22 g (yield: 81%) of the desired compound.

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 15 hours
  4. temperaturecooled
  5. customto precipitate the crystals
  6. temperatureThen, the solution was again cooled slowly
  7. stirringstirred at 10~15° C. for 2 hours
  8. filtrationfiltered
  9. washThe filtered crystal was washed with preheated water(40° C.)
  10. customwas recrystallized
  11. filtrationfiltered
  12. customdried

출처 및 근거

ORD 기록
ord-d9ba63fa0b444ce299a0bfb70e6c7b93
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05922871

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