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Water → HCID 18357788、化合物

HRID 427985
ノート
印刷プレビュー

反応式

HRID 427985 の反応式
[H-].[Na+].[CH3:3][C:4]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:5]=1[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH:14]([OH:19])[C:15]([O:17][CH3:18])=[O:16].[CH3:25]I.O>CN(C)C=O>[CH3:3][C:4]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:5]=1[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH:14]([O:19][CH3:25])[C:15]([O:17][CH3:18])=[O:16].[CH3:3][C:4]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:5]=1[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH:14]([OH:19])[C:15]([O:17][CH3:18])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 18357788HCID 18357788、化合物

生成物 2

HCID 11781996HCID 11781996、化合物HCID 18357788HCID 18357788、化合物収率 191.4%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

60% oily sodium hydride (0.13 g, 3.3 mmol) was added to a solution of methyl 2-[2-(2,5-dimethylphenoxymethyl)-phenyl]-2-hydroxyacetate (0.72 g, 2.4 mmol) and methyl iodide (0.68 g, 4.8 mmol) in N,N-dimethylformamide (6 ml) at 0° C. with stirring. After 30 minutes, ice and water were added in this order, and the mixture was extracted with ethyl acetate, washed successively with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=9/1) to give the desired compound methyl 2-[2-(2,5-dimethylphenoxymethyl)phenyl]-2-hydroxyacetate (0.69 g, 92%) as an oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed successively with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=9/1)

出典と根拠

ORDレコード
ord-d9d47b05693345d096b01108040c9a0e
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06313150B1

反応ノート

読み込み中…

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