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Trifluoroacetic acid → HCID 89783772, 화합물

HRID 1055862
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HRID 1055862 반응식
[CH2:1]([NH:3][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[CH3:2].Cl[C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[C:14]([C:21]3[NH:29][C:28]4[CH2:27][CH2:26][NH:25][C:24](=[O:30])[C:23]=4[CH:22]=3)[CH:15]=[CH:16][CH:17]=2)[N:12]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].C(O)(C(F)(F)F)=O>C1COCC1.CS(C)=O>[CH2:1]([N:3]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[C:11]1[CH:20]=[CH:19][C:18]2[C:13](=[C:14]([C:21]3[NH:29][C:28]4[CH2:27][CH2:26][NH:25][C:24](=[O:30])[C:23]=4[CH:22]=3)[CH:15]=[CH:16][CH:17]=2)[N:12]=1)[CH3:2]
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참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 2724254Sodium bis(trimethylsilyl)amide2회HCID 11804744N-ethylpyridin-3-amineHCID 897835482-(2-chloroquinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one

생성물 1

HCID 89783772HCID 89783772, 화합물수율 11%

시약·촉매·용매 2

HCID 679
Dimethyl Sulfoxide
용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of N-ethylpyridin-3-amine (Enamine, Kiev, Ukraine; 0.164 g, 1.343 mmol) and 2-(2-chloroquinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (Example 1; 0.080 g, 0.269 mmol) was added NaHMDS (1.0 M in THF; 1.343 ml, 1.343 mmol). The dark red reaction was stirred for 30 min, then 0.5 mL 1.0 M NaHMDS in THF was added. After 30 min, the reaction was concentrated in vacuo and 2.5 mL DMSO and TFA (0.207 ml, 2.69 mmol) were added. Purified by rpHPLC (Phenomenex Gemini 150×30 mm C18 column, 5-60% ACN/H2O with 0.1% TFA); product-containing fractions were treated with saturated aq. NaHCO3 and DCM. The organic layer was separated, and the aq. layer was extracted 3×DCM. The combined organic layers were then dried over Na2SO4, filtered, and concentrated in vacuo to give 2-(2-(ethyl(pyridin-3-yl)amino)quinolin-8-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (0.011 g, 0.029 mmol, 11% yield) as a solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 11.97 (1H, br. s), 8.63-8.69 (1H, m), 8.55-8.62 (1H, m), 8.08 (1H, d, J=9.2 Hz), 7.99 (1H, dt, J=7.5, 0.7 Hz), 7.88 (1H, dt, J=8.2, 2.1 Hz), 7.53-7.63 (2H, m), 7.29 (1H, t, J=7.6 Hz), 6.99-7.07 (1H, m), 6.90-6.97 (2H, m), 4.11 (2H, q, J=7.0 Hz), 3.37-3.45 (2H, m), 2.66 (2H, t, J=6.9 Hz), 1.30 (3H, t, J=7.1 Hz). m/z (ESI, +ve) 384.2 (M+H)+.

후처리

  1. customThe dark red reaction
  2. waitAfter 30 min
  3. additionwere added
  4. customPurified by rpHPLC (Phenomenex Gemini 150×30 mm C18 column, 5-60% ACN/H2O with 0.1% TFA)
  5. additionproduct-containing fractions were treated with saturated aq. NaHCO3 and DCM
  6. customThe organic layer was separated
  7. extractionthe aq. layer was extracted 3×DCM
  8. dry with materialThe combined organic layers were then dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-88d2da4742ea43f992db3173f3a99c4a
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394297B2

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