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Methyl iodide → HCID 68006317, 화합물

HRID 1026601
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HRID 1026601 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][C:8](=[O:25])[N:9]2[CH:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)=[N:4][CH:3]=1.[H-].[Na+].[C:28](=O)([O:32]CC)[O:29][CH2:30][CH3:31].[CH3:36]I>O.O1CCCC1>[C:21]([O:20][C:18]([N:15]1[CH2:16][CH2:17][CH:12]([N:9]2[C:10]3[C:5](=[N:4][CH:3]=[C:2]([Cl:1])[CH:11]=3)[CH2:6][C:7]([CH3:36])([C:28]([O:29][CH2:30][CH3:31])=[O:32])[C:8]2=[O:25])[CH2:13][CH2:14]1)=[O:19])([CH3:22])([CH3:24])[CH3:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 68006101HCID 68006101, 화합물

생성물 1

HCID 68006317HCID 68006317, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
70 °C

실험 절차

To a tetrahydrofuran solution (10 ml) of tert-butyl 4-(7-chloro-2-oxo-3,4-dihydro-1,5-naphthyridin-1(2H)-yl)piperidine-1-carboxylate (Reference Example 9-3) (500 mg) were added at 0° C. sodium hydride (161 mg) and diethyl carbonate (0.66 ml). After the reaction solution was stirred at 70° C. for 4 hours, methyl iodide (0.171 ml) was added at 0° C., and stirred at room temperature for 6 hours. Water was added to the reaction solution at 0° C., and extracted with ethyl acetate. The collected organic layer was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to afford ethyl 1-[1-(tert-butoxycarbonyl)piperidin-4-yl]-7-chloro-3-methyl-2-oxo-1,2,3,4-tetrahydro-1,5-naphthyridine-3-carboxylate (286 mg).

후처리

  1. stirringstirred at room temperature for 6 hours
  2. extractionextracted with ethyl acetate
  3. washThe collected organic layer was washed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5ab51403f85043b695cb61c7829a27f5
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729095B2

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