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Methyl iodide → HCID 22494028、化合物

HRID 1296208
ノート
印刷プレビュー

反応式

HRID 1296208 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22494074HCID 22494074、化合物

生成物 1

HCID 22494028HCID 22494028、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-47eec69980a54609a0725dc6bb7a8670
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07244861B2

反応ノート

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