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Methyl iodide → HCID 22494028, 화합물

HRID 1296208
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HRID 1296208 반응식
[CH2:1]([O:3][C:4](=[O:28])[CH:5]([O:24][CH:25]([CH3:27])[CH3:26])[CH2:6][C:7]1[CH:12]=[C:11]([CH2:13][NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:10]([OH:22])=[C:9]([Br:23])[CH:8]=1)[CH3:2].IC.[C:31](=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:28])[CH:5]([O:24][CH:25]([CH3:27])[CH3:26])[CH2:6][C:7]1[CH:12]=[C:11]([CH2:13][NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:10]([O:22][CH3:31])=[C:9]([Br:23])[CH:8]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22494074HCID 22494074, 화합물

생성물 1

HCID 22494028HCID 22494028, 화합물수율 90.1%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

944 mg of 3-(3-bromo-5-[(t-butoxycarbonyl)amino]methyl-4-hydroxyphenyl)-2-isopropoxypropionic acid ethyl ester was dissolved in 5 ml of N,N-dimethylformamide, and 0.15 ml of iodomethane and 500 mg of potassium carbonate were successively added, followed by stirring for 2 hours at room temperature. Then, the reaction mixture was diluted with ethyl acetate, and the organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography, to give 876 mg of 3-(3-bromo-5-[(t-butoxycarbonyl)amino]methyl-4-methoxyphenyl)-2-isopropoxypropionic acid ethyl ester from fractions eluted with hexane-ethyl acetate (4:1).

후처리

  1. washthe organic layer was washed with water and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-47eec69980a54609a0725dc6bb7a8670
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07244861B2

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