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Cesium carbonate → HCID 178458755, 화합물

HRID 2271532
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HRID 2271532 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][C:6]([C:12](=[O:15])[CH2:13][CH3:14])=[C:5]2Cl.C(O)(=O)C.C(O)(=O)C.[CH3:25][N:26]([CH2:28][C@H:29]1[CH2:34][CH2:33][C@H:32]([NH2:35])[CH2:31][CH2:30]1)[CH3:27].C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.CN(C=O)C.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][C:6]([C:12](=[O:15])[CH2:13][CH3:14])=[C:5]2[NH:35][C@H:32]1[CH2:33][CH2:34][C@H:29]([CH2:28][N:26]([CH3:27])[CH3:25])[CH2:30][CH2:31]1
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참가 물질

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HCID 10796Cesium carbonateHCID 866928451-(6-Bromo-4-chloroquinolin-3-yl)propan-1-oneHCID 178476567HCID 178476567, 화합물

생성물 1

HCID 178458755HCID 178458755, 화합물수율 58%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 8857
Ethyl Acetate
용매
HCID 312751,4-Dioxane용매

실험 절차

To a suspension of 1-(6-bromo-4-chloroquinolin-3-yl)propan-1-one (500 mg, 1.67 mmol) in dioxane (10 mL) and DMF (4 mL) was added trans-4-((dimethylamino)methyl)cyclohexanamine diacetic acid salt (583 mg, 2.11 mmol) and Cs2CO3 (3.27 g, 10.0 mmol). The resultant suspension was then heated to 90° C. and stirred for 5.5 h. The reaction mixture was cooled to room temperature and diluted with ethyl acetate. The solution was then washed with saturated sodium bicarbonate, water and then brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. Purification by column chromatography (silica, 0-10% methanol/dichloromethane) afforded the desired product (403 mg, 58%) as a tan solid. 1H NMR (300 MHz, CDCl3) δ 10.79 (d, J=8.4 Hz, 1H), 9.00 (s, 1H), 8.27 (d, J=2.0 Hz, 1H), 7.83-7.67 (m, 2H), 4.01-3.88 (m, 1H), 3.08 (q, J=7.2 Hz, 2H), 2.24 (s, 6H), 2.21-2.12 (m, 2H), 1.98 (d, J=13.4 Hz, 2H), 1.61-1.42 (m, 3H), 1.25 (t, J=7.3 Hz, 3H), 1.19-1.00 (m, 2H).

후처리

  1. washThe solution was then washed with saturated sodium bicarbonate, water
  2. dry with materialbrine, dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customPurification by column chromatography (silica, 0-10% methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-38e508ac79984bc19c7273a2743af9d3
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120749B2

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