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Methyl iodide → HCID 69907754、化合物

HRID 618133
ノート
印刷プレビュー

反応式

HRID 618133 の反応式
[C:1]([NH:4][C:5]1[CH:13]=[C:12]2[C:8]([C:9](/[CH:14]=[C:15](\[S:30][CH2:31][CH:32]([OH:35])[CH2:33][OH:34])/[C:16]([C:18]3[CH:23]=[C:22]([O:24][CH3:25])[C:21]([O:26][CH3:27])=[C:20]([O:28][CH3:29])[CH:19]=3)=[O:17])=[CH:10][NH:11]2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[CH3:36]I.[H-].[Na+]>CN(C)C=O.O1CCCC1>[C:1]([NH:4][C:5]1[CH:13]=[C:12]2[C:8]([C:9](/[CH:14]=[C:15](\[S:30][CH2:31][CH:32]([OH:35])[CH2:33][OH:34])/[C:16]([C:18]3[CH:23]=[C:22]([O:24][CH3:25])[C:21]([O:26][CH3:27])=[C:20]([O:28][CH3:29])[CH:19]=3)=[O:17])=[CH:10][N:11]2[CH3:36])=[CH:7][CH:6]=1)(=[O:3])[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 24758Sodium hydrideHCID 69907738HCID 69907738、化合物

生成物 1

HCID 69907754HCID 69907754、化合物収率 81%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 125 (300.0 mg) obtained in Example 125 was dissolved in a mixed solvent of N,N-dimethylformamide and tetrahydrofuran (1:1), and methyl iodide (93.6 mg) and then sodium hydride (26.4 mg, 60% mineral oil dispersion) were added thereto, followed by stirring for 1.5 hours. The reaction solution was subjected to partitioning between chloroform and water, and the organic layer was successively washed with water and a saturated saline, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crude crystals were washed with chloroform and recrystallized from a mixed solvent of ethanol, N,N-dimethylformamide, and water to give Compound 126 (249.7 mg).

後処理

  1. customto partitioning between chloroform and water
  2. washthe organic layer was successively washed with water
  3. dry with materiala saturated saline, dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained crude crystals
  6. washwere washed with chloroform
  7. customrecrystallized from a mixed solvent of ethanol, N,N-dimethylformamide, and water

出典と根拠

ORDレコード
ord-d110662bdc174f148fdae9c736e1887c
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05952355

反応ノート

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