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4-Methoxybenzylamine → 1-[6-(4-Methoxy-benzylamino)-1H-pyrrolo[2,3-b]pyridin-3-yl]-ethanone

HRID 1527260
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HRID 1527260 반응식
Cl[C:2]1[N:7]=[C:6]2[NH:8][CH:9]=[C:10]([C:11](=[O:13])[CH3:12])[C:5]2=[CH:4][CH:3]=1.CC(C1C=C(C(C)C)C(C2C(P(C3CCCCC3)C3CCCCC3)=C(OC)C=CC=2OC)=C(C(C)C)C=1)C.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[CH3:62][O:63][C:64]1[CH:71]=[CH:70][C:67]([CH2:68][NH2:69])=[CH:66][CH:65]=1>CC(C1C=C(C(C)C)C(C2C(P(C3CCCCC3)C3CCCCC3)=C(OC)C=CC=2OC)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+]>[CH3:62][O:63][C:64]1[CH:71]=[CH:70][C:67]([CH2:68][NH:69][C:2]2[N:7]=[C:6]3[NH:8][CH:9]=[C:10]([C:11](=[O:13])[CH3:12])[C:5]3=[CH:4][CH:3]=2)=[CH:66][CH:65]=1
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참가 물질

6

반응물 4

HCID 754524-MethoxybenzylamineHCID 2733832Lithium hexamethyldisilazaneHCID 25112535BrettphosHCID 717210681-(6-Chloro-1H-pyrrolo[2,3-b]pyridin-3-yl)ethanone

생성물 1

HCID 682841881-[6-(4-Methoxy-benzylamino)-1H-pyrrolo[2,3-b]pyridin-3-yl]-ethanone

시약·촉매·용매 1

HCID 25112666
BrettPhos Palladacycle
촉매

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온도
65 °C

실험 절차

The reaction was performed according to the protocol described in Org. Lett., 2010, 12(20), 4438-4441. A vial containing 1-(6-chloro-1H-pyrrolo[2,3-b]pyridin-3-yl)-ethanone (100 mg, 0.49 mmol), BrettPhos (2.62 mg, 4.88 μmol) and BrettPhos precatalyst (3.9 mg, 4.88 μmol) and a magnetic stir bar was sealed with a teflon screw-cap, evacuated and backfilled with argon. A balloon of argon was placed on top of the vial, to allow a pressure balance and LiHMDS (1 M in THF, 1172 μL, 1.17 mmol) was added, followed by 4-methoxybenzylamine (76 μL, 0.59 mmol). The reaction mixture was stirred and heated at 65° C. for 22 h, then allowed to cool to RT, quenched by the addition of 1 M HCl (1 mL) diluted with EtOAc and poured into a saturated aqueous solution of NaHCO3. After extracting twice with EtOAc, the combined organic layers were washed with brine, dried (Na2SO4), filtered and concentrated. The crude was purified by flash column chromatography on silica gel (c-hexane to EtOAc). TLC, Rf (EtOAc)=0.75; MS (UPLC/MS): 296.2 [M+H]+, 591.3 [2M+H]+, 613.2 [2M+Na]+; tR (HPLC conditions f): 1.5 min.

후처리

  1. customscrew-cap
  2. customevacuated
  3. additionwas added
  4. temperatureto cool to RT
  5. customquenched by the addition of 1 M HCl (1 mL)
  6. additiondiluted with EtOAc
  7. additionpoured into a saturated aqueous solution of NaHCO3
  8. extractionAfter extracting twice with EtOAc
  9. washthe combined organic layers were washed with brine
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customThe crude was purified by flash column chromatography on silica gel (c-hexane to EtOAc)
  14. custom1.5 min.

출처 및 근거

ORD 기록
ord-c4ea305c38b34699a189b969a4b8a0b8
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09085555B2

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