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Ammonia → HCID 66604465, 화합물

HRID 2410863
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HRID 2410863 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([CH2:8][N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[N:6][CH:7]=1.CC1(C)C(C)(C)OB(B2OC(C)(C)C(C)(C)O2)O1.CC([O-])=O.[K+].Br[C:39]1[CH:40]=[C:41]([C:58]([NH2:60])=[O:59])[C:42]2[NH:43][C:44]3[CH:45]=[C:46]([N:52]4[CH2:57][CH2:56][O:55][CH2:54][CH2:53]4)[CH:47]=[CH:48][C:49]=3[C:50]=2[N:51]=1.CC1(C)C(C)(C)OB(C2C=CC(CN3CCOCC3)=NC=2)O1.C([O-])([O-])=O.[Na+].[Na+].C(O)(C(F)(F)F)=O.N>CO.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.O.COCCOC>[O:55]1[CH2:56][CH2:57][N:52]([C:46]2[CH:47]=[CH:48][C:49]3[C:50]4[N:51]=[C:39]([C:2]5[CH:7]=[N:6][C:5]([CH2:8][N:9]6[CH2:14][CH2:13][O:12][CH2:11][CH2:10]6)=[CH:4][CH:3]=5)[CH:40]=[C:41]([C:58]([NH2:60])=[O:59])[C:42]=4[NH:43][C:44]=3[CH:45]=2)[CH2:53][CH2:54]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

13

반응물 8

HCID 222AmmoniaHCID 6422Trifluoroacetic acid2회HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 120852844-((5-Bromopyridin-2-yl)methyl)morpholineHCID 57416470
4-{[5-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl]methyl}morpholine
HCID 86663061HCID 86663061, 화합물

생성물 1

HCID 66604465HCID 66604465, 화합물수율 35.7%

시약·촉매·용매 4

HCID 178418807HCID 178418807, 화합물촉매2회HCID 887Methanol용매3회HCID 962Water용매2회HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
100 °C

실험 절차

A microwave vial containing a mixture of 4-((5-bromopyridin-2-yl)methyl)morpholine (537 mg, 2.09 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (583 mg, 2.30 mmol), KOAc (410 mg, 4.18 mmol) and PdCl2(dppf)-CH2Cl2 adduct (85 mg, 0.10 mmol) was flushed with nitrogen, dioxane (5 mL) was added. and the vial was sealed and heated at 100° C. for 6 hr. The reaction was filtered and the solid was washed with EtOAc. The filtrate was and washed with water, brine, and dried over MgSO4. Removal of the solvent left 750 mg of crude 4-((5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl)methyl)morpholine (750 mg) as a brown thick oil that was used as such. A microwave vial containing a mixture of 2-bromo-7-morpholino-5H-pyrido[3,2-b]indole-4-carboxamide (60 mg, 0.14 mmol), 4-((5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl)methyl)morpholine (130 mg, 0.171 mmol), PdCl2(dppf)-CH2Cl2 adduct (12 mg, 0.014 mmol) was flushed with nitrogen. DME (2.5 mL) and Na2CO3 (0.36 mL, 0.72 mmol, 2.0 M aq. solution) were added and the vial was sealed and heated at 100° C. for 5 hr. Preparative HPLC (100×30 mm Luna C18 column, Solvent A=10% Methanol, 90% H2O, 0.1% TFA; Solvent B=90% Methanol, 10% H2O, 0.1% TFA; gradient of 0 to 60% B over 10 min at 42 mL/min) followed by SCX capture and release with 2 N NH3 in MeOH gave 7-morpholino-2-(6-(morpholinomethyl)pyridin-3-yl)-5H-pyrido[3,2-b]indole-4-carboxamide (25 mg, 0.050 mmol, 35% yield) as a solid. MS (ESI) m/z 473.21 (M+H). 1H NMR (500 MHz, Acetone) δ ppm 10.75 (1H, s), 9.36 (1H, d, J=2.14 Hz), 8.58 (1H, dd, J=8.09, 2.29 Hz), 8.35 (1H, s), 8.10-8.22 (2H, m), 7.62 (1H, d, J=7.93 Hz), 7.29 (1H, d, J=2.14 Hz), 7.18 (1H, br. s.), 7.07 (1H, dd, J=8.85, 2.14 Hz), 3.80-3.87 (4H, m), 3.71 (2H, s), 3.64-3.69 (4H, m), 3.28-3.35 (4H, m), 2.47-2.57 (4H, m).

후처리

  1. additionA microwave vial containing
  2. customwas flushed with nitrogen, dioxane (5 mL)
  3. additionwas added
  4. customand the vial was sealed
  5. filtrationThe reaction was filtered
  6. washthe solid was washed with EtOAc
  7. washwashed with water, brine
  8. dry with materialdried over MgSO4
  9. customRemoval of the solvent
  10. waitleft 750 mg of crude 4-((5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl)methyl)morpholine (750 mg) as a brown thick oil that
  11. additionA microwave vial containing
  12. customwas flushed with nitrogen
  13. customthe vial was sealed
  14. temperatureheated at 100° C. for 5 hr

출처 및 근거

ORD 기록
ord-e26b7a1625024dcd929fb549d604290b
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815840B2

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