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Formic Acid → 1-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-1H-imidazo[4,5-c]quinoline

HRID 1043009
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HRID 1043009 반응식
[CH3:1][C:2]1[C:6]([C:7]2[CH:16]=[C:15]3[C:10]([C:11]([NH:18][CH2:19]C4C=CC=CC=4)=[C:12]([NH2:17])[CH:13]=[N:14]3)=[CH:9][CH:8]=2)=[C:5]([CH3:26])[O:4][N:3]=1.[CH:27]1[CH:28]=[CH:29][C:30]2N(O)N=N[C:31]=2[CH:32]=1.CCN=C=N[CH2:42][CH2:43][CH2:44]N(C)C.[CH3:48]CN(CC)CC.C(O)=O>C(Cl)Cl.O>[C:43]([C:31]1[CH:30]=[CH:29][CH:28]=[CH:27][C:32]=1[N:18]1[C:11]2[C:10]3[CH:9]=[CH:8][C:7]([C:6]4[C:2]([CH3:1])=[N:3][O:4][C:5]=4[CH3:26])=[CH:16][C:15]=3[N:14]=[CH:13][C:12]=2[N:17]=[CH:19]1)([CH3:44])([CH3:48])[CH3:42]
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참가 물질

8

반응물 5

HCID 284Formic AcidHCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 672063207-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine2회

생성물 1

HCID 52934041
1-[2-(tert-butyl)phenyl]-7-(3,5-dimethyl-4-isoxazolyl)-1H-imidazo[4,5-c]quinoline
수율 48.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 7-(3,5-dimethyl-4-isoxazolyl)-N4-(phenylmethyl)-3,4-quinolinediamine (for aq preparation see Intermediate 28, 0.2 g, 0.52 mmol) in DCM (10 ml) were added HOBT (0.081 g, 0.62 mmol), EDCI (0.118 g, 0.62 mmol), Et3N (0.062 g, 0.62 mmol) and formic acid (0.025 g, 0.52 mmol). The reaction mixture was stirred at room temperature overnight, then poured into water and extracted with DCM. The organic phase was washed with water, dried over Na2SO4 and concentrated. The crude solid was re-crystallized from EtOAc to give the title compound as off-white crystals (0.1 g, 48%). M.p: 216° C. 1H NMR (300 MHz, CDCl3, ppm) δ: 9.36 (s, 1H), 8.06 (s, 1H), 8.01 (s, 1H), 7.73 (d, J=7.2 Hz, 1H), 7.56 (dd, J=8.1, 8.1 Hz, 1H), 7.34 (dd, J=7.7, 7.7 Hz, 1H), 7.15-7.06 (m, 2H), 2.36 (s, 3H), 2.23 (s, 3H), 1.07 (s, 9H). LC-HRMS: ES+ exact mass calculated for C25H24N4O: 397.2028 MH+, found: 397.2021, Rt 3.03 min.

후처리

  1. extractionextracted with DCM
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customThe crude solid was re-crystallized from EtOAc

출처 및 근거

ORD 기록
ord-d2bf2ebdc99d4c0885f49984849a8735
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08557984B2

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