Methyl iodide → HCID 59344901, 화합물

HRID 18187

반응식

HRID 18187 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:22]3[O:21][C:20]([C:23](=[O:25])[NH2:24])=[C:19]([CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[C:18]=3[CH:17]=[C:16]([CH3:33])[CH:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[CH3:36]I>CN(C=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[C:22]3[O:21][C:20]([C:23](=[O:25])[NH:24][CH3:36])=[C:19]([CH2:26][C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=4)[C:18]=3[CH:17]=[C:16]([CH3:33])[CH:15]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 593449044-(3-Benzyl-2-carbamoyl-5-methyl-benzofuran-7-yl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 59344901HCID 59344901, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(3-Benzyl-2-carbamoyl-5-methyl-benzofuran-7-yl)-piperazine-1-carboxylic acid tert-butyl ester (0.25 gm, 0.556 mmol) was dissolved in 5 ml DMF and sodium hydride (60% in oil, 0.033 gm, 0.83 mmol) was added, resulting in formation of a precipitate. Methyl iodide (0.052 ml, 0.83 mmol) was added and the solid dissolved to give a clear solution. After one hour the mixture was concentrated under reduced pressure and the residue was purified by preparative thin layer chromatography (3/97 methanol/dichloromethane). One band was again purified (40/60, tetrahydrofuran/hexane) to give 4-(3-Benzyl-5-methyl-2-methylcarbamoyl-benzofuran-7-yl)-piperazine-1-carboxylic acid tert-butyl ester. A second band was recrystallized from acetonitrile to give 4-(3-Benzyl-2-dimethylcarbamoyl-5-methyl-benzofuran-7-yl)-piperazine-1-carboxylic acid tert-butyl ester.

후처리

  1. customresulting in formation of a precipitate
  2. dissolutionthe solid dissolved
  3. customto give a clear solution
  4. concentrationAfter one hour the mixture was concentrated under reduced pressure
  5. customthe residue was purified by preparative thin layer chromatography (3/97 methanol/dichloromethane)
  6. customOne band was again purified (40/60, tetrahydrofuran/hexane)

출처 및 근거

ORD 기록
ord-61353783fe484b70a1b31bc4c53192dc
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741326B2

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