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HCID 68810823, 화합물 → HCID 9842488, 화합물

HRID 1790857
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HRID 1790857 반응식
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[CH:16][CH:17]=[C:18]3[C:23]=2[N:22]=[C:21]([N:24]2[C:28]4[CH:29]=[CH:30][C:31]([O:33][CH3:34])=[CH:32][C:27]=4[N:26]=[CH:25]2)[CH:20]=[CH:19]3)[CH2:10][CH2:9]1)(C)(C)C>FC(F)(F)C(O)=O>[CH3:34][O:33][C:31]1[CH:30]=[CH:29][C:28]2[N:24]([C:21]3[CH:20]=[CH:19][C:18]4[C:23](=[C:14]([N:11]5[CH2:10][CH2:9][CH:8]([NH2:7])[CH2:13][CH2:12]5)[CH:15]=[CH:16][CH:17]=4)[N:22]=3)[CH:25]=[N:26][C:27]=2[CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 68810823HCID 68810823, 화합물

생성물 1

HCID 9842488HCID 9842488, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

{1-[2-(5-Methoxy-benzoimidazol-1-yl)-quinolin-8-yl]-piperidin-4-yl}-carbamic acid tert-butyl ester G (8.40 g, 17.7 mmol) was dissolved in 50 mL of trifluoroacetic acid (TFA) under an atmosphere of dry N2. The reaction mixture was stirred at ambient temperature for 15 minutes after which time it was concentrated under vacuum to give a yellow oil. The oil was partitioned between DCM and 0.1N aqueous NaOH. The DCM layer was washed again with 0.1N aqueous NaOH. The DCM layer was dried over Na2SO4, filtered and concentrated to give 5.85 g of 1-[2-(5-Methoxy-benzoimidazol-1-yl)-quinolin-8-yl]-piperidin-4-ylamine as a yellow solid. C.I. m/z 374 [M+1]; 1H NMR (CDCl3) δ 8.66 (s, 1 H), 8.37 (d, J=8.9 Hz, 1 H), 8.30 (d, J=8.7 Hz, 1 H), 7.68 (d, J=8.9 Hz, 1 H), 7.47 (m, 2 H), 7.35 (d, J=2.3 Hz, 1 H), 7.25 (m, 1 H), 7.06 (dd, J=2.5, 8.9 Hz, 1 H), 3.91 (s, 3 H), 3.88 (m, 2 H), 2.90 (m, 3 H), 2.05 (m, 2 H), 1.83 (m, 2 H), 1.50 (brs, 2 H).

후처리

  1. concentrationwas concentrated under vacuum
  2. customto give a yellow oil
  3. customThe oil was partitioned between DCM and 0.1N aqueous NaOH
  4. washThe DCM layer was washed again with 0.1N aqueous NaOH
  5. dry with materialThe DCM layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-067c9c222567442b89d655c5c7c1f3c7
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07071337B2

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