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Methyl iodide → HCID 68418565, 화합물

HRID 20225
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HRID 20225 반응식
[H-].[Na+].[O:3]=[C:4]1[NH:8][CH2:7][CH2:6][N:5]1[CH:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH2:11][CH2:10]1.[CH3:25]I>CN(C=O)C>[CH3:25][N:8]1[CH2:7][CH2:6][N:5]([CH:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH2:13][CH2:14]2)[C:4]1=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 23463818Benzyl 4-(2-oxoimidazolidin-1-yl)piperidine-1-carboxylate

생성물 1

HCID 68418565HCID 68418565, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (80 mg) was added to a solution of benzyl 4-(2-oxoimidazolidin-1-yl)piperidin-1-carboxylate (0.30 g) in DMF (5 mL), the mixture was stirred at room temperature for 30 minutes. After addition of methyl iodide (0.25 mL), the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, diluted with water, and extracted with ethyl acetate. The extract was washed with water, an aqueous 5% citric acid solution and saturated saline solution and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain the title compound (0.32 g, quantitative) as a colorless oil.

후처리

  1. stirringthe mixture was stirred at room temperature for 15 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additiondiluted with water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialan aqueous 5% citric acid solution and saturated saline solution and dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-ea29079ca2424189abc014472852b2d0
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745623B2

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