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Sodium Chloride → N-((6-amino-2-methylpyridin-3-yl)methyl)-1-((2-methylquinolin-6-yl)methyl)-1H-pyrazole-4-carboxamide

HRID 928442
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HRID 928442 반응식
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH2:12][N:13]3[CH:17]=[C:16]([C:18]([OH:20])=O)[CH:15]=[N:14]3)[CH:8]=2)[N:3]=1.[Na+].[Cl-].CCN=C=NCCCN(C)C.Cl.C1C=NC2N(O)N=NC=2C=1.CN1CCOCC1.[NH2:52][CH2:53][C:54]1[CH:55]=[CH:56][C:57]([NH2:61])=[N:58][C:59]=1[CH3:60]>CN(C=O)C.CO.C(#N)C>[NH2:61][C:57]1[N:58]=[C:59]([CH3:60])[C:54]([CH2:53][NH:52][C:18]([C:16]2[CH:15]=[N:14][N:13]([CH2:12][C:7]3[CH:8]=[C:9]4[C:4](=[CH:5][CH:6]=3)[N:3]=[C:2]([CH3:1])[CH:11]=[CH:10]4)[CH:17]=2)=[O:20])=[CH:55][CH:56]=1
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참가 물질

10

반응물 6

HCID 5234Sodium ChlorideHCID 79724-MethylmorpholineHCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 101977255-(Aminomethyl)-6-methylpyridin-2-amineHCID 580812841-((2-methylquinolin-6-yl)methyl)-1H-pyrazole-4-carboxylic acid

생성물 1

HCID 66723582
N-((6-amino-2-methylpyridin-3-yl)methyl)-1-((2-methylquinolin-6-yl)methyl)-1H-pyrazole-4-carboxamide

시약·촉매·용매 3

HCID 887Methanol용매2회HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매

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온도
50 °C

실험 절차

To a suspension of 1-((2-methylquinolin-6-yl)methyl)-1H-pyrazole-4-carboxylic acid (incl. NaCl) (100 mg, 0.337 mmol), EDC.HCl (84 mg, 0.438 mmol) and HOAt (59.6 mg, 0.438 mmol) in DMF (1 ml) was added N-methylmorpholine (0.185 ml, 1.684 mmol). The reaction mixture was stirred for 1 h at 50° C., then 5-(aminomethyl)-6-methylpyridin-2-amine (70.7 mg, 0.337 mmol) was added. Stirring continued at 50° C. for 18 h. Reaction mixture was diluted with methanol, then applied onto a PL-SO3H cartridge (500 mg/6 ml by VARIAN) to catch the desired amine product, washed the cartridge with DMF, DCM and MeOH to remove all impurities, then the product was released from the cartridge by washing with 2M NH3 in MeOH. The basic filtrate was evaporated to give the crude material, which was treated with 0.2 ml of MeOH and 1 ml of ACN in ultrasonic bath. The precipitate formed was filtered, washed with 1 ml of ACN and dried under high vacuum for 4 days to yield the title compound. HPLC (Method J) Rt=2.373 min, MS (Method V) [M+H]+=387.1.

후처리

  1. stirringStirring
  2. waitcontinued at 50° C. for 18 h
  3. customReaction mixture
  4. washwashed the cartridge with DMF, DCM and MeOH
  5. customto remove all impurities
  6. washby washing with 2M NH3 in MeOH
  7. customThe basic filtrate was evaporated
  8. customto give the crude material, which
  9. customThe precipitate formed
  10. filtrationwas filtered
  11. washwashed with 1 ml of ACN
  12. customdried under high vacuum for 4 days

출처 및 근거

ORD 기록
ord-1eee77baa79a4995a82d67ed559d2e14
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290485B2

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