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Methyl iodide → HCID 20145193, 화합물

HRID 648658
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HRID 648658 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH:12]([C:24]([NH2:26])=[O:25])[C:13]2[CH:23]=[CH:22][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:15][CH:14]=2)[CH2:9][CH2:10][CH3:11])=[C:4]([N:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)[CH:3]=1.[H-].[Na+].[CH3:35]I>CN(C)C=O>[CH3:35][O:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH:12]([C:24]([NH2:26])=[O:25])[C:13]2[CH:14]=[CH:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:22][CH:23]=2)[CH2:9][CH2:10][CH3:11])=[C:4]([N:27]2[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32]2)[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20145211HCID 20145211, 화합물

생성물 1

HCID 20145193HCID 20145193, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

A solution of 5.0 gm (11.4 m mol) of ethyl 4-[(1-(4-hydroxy-2-piperidino-phenyl)-1-butyl)-aminocarbonylmethyl]-benzoate in 45 ml of absolute dimethylformamide was added dropwise, under stirring, at ambient temperature, to 548 mg (11.4 m mol) of sodium hydride (50% in oil) in 10 ml of absolute dimethylformamide. The mixture was stirred for a further 15 minutes, and then a solution of 0.71 ml (11.4 m mol) of methyliodide in 8 ml of absolute dimethylformamide was slowly added thereto dropwise. The mixture was stirred for a further two and one-half hours at ambient temperature, evaporated in vacuo, and distributed between water and ether. The ether phase was dried, filtered, and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silica gel [toluene/acetone (20:1)].

후처리

  1. stirringThe mixture was stirred for a further two and one-half hours at ambient temperature
  2. customevaporated in vacuo
  3. dry with materialThe ether phase was dried
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation in vacuo
  6. customThe evaporation residue was purified by column chromatography on silica gel [toluene/acetone (20:1)]

출처 및 근거

ORD 기록
ord-b3f67891bee54941ae2fd8e9ae0d6fb6
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04735959

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