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Acetone → HCID 44198125, 화합물

HRID 79619
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HRID 79619 반응식
[NH2:1][CH2:2][CH2:3][C:4]([N:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:17]([Br:18])=[CH:16][N:15]=[C:14]3[NH:19][CH:20]=[C:21]([NH:22][C:23](=[O:30])[C:24]4[CH:29]=[CH:28][CH:27]=[N:26][CH:25]=4)[C:13]=23)[CH2:8][CH2:7]1)=[O:5].[CH3:31][C:32]([CH3:34])=O.CCN(C(C)C)C(C)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+].Cl>C(Cl)Cl.CCOCC.CN(C=O)C.ClCCCl>[Br:18][C:17]1[C:12]([N:9]2[CH2:8][CH2:7][N:6]([C:4](=[O:5])[CH2:3][CH2:2][NH:1][CH:32]([CH3:34])[CH3:31])[CH2:11][CH2:10]2)=[C:13]2[C:21]([NH:22][C:23](=[O:30])[C:24]3[CH:29]=[CH:28][CH:27]=[N:26][CH:25]=3)=[CH:20][NH:19][C:14]2=[N:15][CH:16]=1
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참가 물질

11

반응물 6

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 44198124N-(4-(4-(3-aminopropanoyl)piperazin-1-yl)-5-bromo-1H-pyrrolo[2,3-b]pyri din-3-yl)nicotinamide

생성물 1

HCID 44198125
HCID 44198125, 화합물
수율 56.6%

시약·촉매·용매 4

HCID 111,2-Dichloroethane용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

N-(4-(4-(3-aminopropanoyl)piperazin-1-yl)-5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)nicotinamide (0.060 g, 0.103 mmol, see Example 62) and acetone (0.0599 g, 1.03 mmol) were placed in 1:1 DCE:DMF (5 mL). DIEA (d 0.742; 0.0898 mL, 0.516 mmol) was then added, followed by the addition of NaBH(OAc)3 (0.0437 g, 0.206 mmol). The reaction was then stirred for 30 minutes, and poured into Na2CO3 and extracted into DCM (3×30 mL). The organic fractions were combined, dried, filtered and concentrated. The resulting residue was purified by reverse phase HPLC to give a pure product. The product was then dissolved in minimal DCM and added to a stirring solution of 1M HCl in ether (10 mL). The resulting solid was collected to give N-(5-bromo-4-(4-(3-(isopropylamino)propanoyl)piperazin-1-yl)-1H-pyrrolo[2,3-b]pyridin-3-yl)nicotinamide (0.030 g, 46.6% yield) as the trihydrochloride salt. MS APCI (+) m/z 515 detected.

후처리

  1. extractionextracted into DCM (3×30 mL)
  2. customdried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe resulting residue was purified by reverse phase HPLC
  6. customto give a pure product
  7. customThe resulting solid was collected

출처 및 근거

ORD 기록
ord-0d7d6730ec534694ad6f2359f5cf163b
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841304B2

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