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Sodium Hydroxide → HCID 68157525, 화합물

HRID 1520929
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HRID 1520929 반응식
[CH3:1][CH:2]([CH3:31])[CH2:3][CH:4]([NH:20][C:21]1[CH:30]=[CH:29][C:24]([C:25](OC)=[O:26])=[CH:23][N:22]=1)[C:5]1[CH:6]=[N:7][C:8]([N:11]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[N:12]2)=[CH:9][CH:10]=1.[OH-].[Na+].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C.Cl.[NH2:68][CH2:69][CH2:70][C:71]([O:73][CH3:74])=[O:72]>CO.[Cl-].[Na+].O>[CH3:1][CH:2]([CH3:31])[CH2:3][CH:4]([NH:20][C:21]1[CH:30]=[CH:29][C:24]([C:25]([NH:68][CH2:69][CH2:70][C:71]([O:73][CH3:74])=[O:72])=[O:26])=[CH:23][N:22]=1)[C:5]1[CH:6]=[N:7][C:8]([N:11]2[CH:15]=[C:14]([C:16]([F:17])([F:19])[F:18])[CH:13]=[N:12]2)=[CH:9][CH:10]=1
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참가 물질

8

반응물 5

HCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 2734767Methyl 3-aminopropanoate hydrochlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68178642HCID 68178642, 화합물

생성물 1

HCID 68157525
HCID 68157525, 화합물
수율 91.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 57417360Sodium chloride; water용매

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온도
20 °C

실험 절차

To a solution of (+/−)-methyl 6-(3-methyl-1-(6-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyridin-3-yl)butylamino)nicotinate (800 mg, 1.85 mmol) in methanol (5 mL) was added 2N aqueous sodium hydroxide (9.2 mL, 18.4 mmol). The resulting mixture was stirred at 20° C. for 2 h. Methanol was removed under reduced pressure and the residue was acidified by addition of 1N aqueous HCl to pH 3-4 and extracted with dichloromethane (30 mL×2). The combined organic layers were concentrated under reduced pressure. The residue was dissolved in DMF (10 mL). HATU (1.36 mg, 3.58 mmol) and N,N-di-iso-propylethylamine (1.15 mg, 8.95 mmol) were added. Methyl 3-aminopropanoate hydrochloride (370 mg, 2.68 mmol) was added. The resulting mixture was stirred at 30° C. for 1 h. The mixture was poured into brine (30 mL) and extracted with ethyl acetate (30 mL×2). The combined organic layers were washed with 1N aqueous HCl (30 mL), dried over anhydrous Na2SO4 and concentrated to dryness. The crude residue was purified silica gel chromatography to give (+/−)-methyl 3-(6-(3-methyl-1-(6-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyridin-3-yl)butylamino)nicotinamido)propanoate (850 mg) as an oil. 1H NMR (400 MHz, CDCl3) δ 8.75 (s, 1H), 8.37 (d, J=12.0 Hz, 2H), 7.87 (d, J=8.4 Hz, 1H), 7.80 (s, 1H), 7.76-7.70 (m, 2H), 6.52 (s, 1H), 6.22 (d, J=8.4 Hz, 1H), 5.07 (d, J=4.0 Hz, 1H), 4.86 (d, J=9.2 Hz, 1H), 3.62-3.58 (m, 5H), 2.54 (t, J=5.6 Hz, 2H), 1.77-1.59 (m, 3H), 1.75-1.63 (m, 2H), 0.95 (d, J=6.0 Hz, 3H), 0.91 (d, J=6.0 Hz, 3H).

후처리

  1. customMethanol was removed under reduced pressure
  2. additionthe residue was acidified by addition of 1N aqueous HCl to pH 3-4
  3. extractionextracted with dichloromethane (30 mL×2)
  4. concentrationThe combined organic layers were concentrated under reduced pressure
  5. dissolutionThe residue was dissolved in DMF (10 mL)
  6. stirringThe resulting mixture was stirred at 30° C. for 1 h
  7. extractionextracted with ethyl acetate (30 mL×2)
  8. washThe combined organic layers were washed with 1N aqueous HCl (30 mL)
  9. dry with materialdried over anhydrous Na2SO4
  10. concentrationconcentrated to dryness
  11. customThe crude residue was purified silica gel chromatography

출처 및 근거

ORD 기록
ord-6006867d9e8d4decbf104e9eb42a274b
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073871B2

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