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Water → HCID 20513506、化合物

HRID 1164023
ノート
印刷プレビュー

反応式

HRID 1164023 の反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:17][C:18]#N.[H-].[Na+].[CH3:22]I.O.C[N:26]([CH3:29])C=O>>[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])=[CH:7][CH:6]=[CH:5][C:4]=1[C:17]([CH3:18])([CH3:22])[C:29]#[N:26]
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 5

HCID 962WaterHCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20513415HCID 20513415、化合物

生成物 1

HCID 20513506HCID 20513506、化合物

実験手順

A solution of 2-[2-methoxy-3-(o-tolyloxy)phenyl]acetonitrile (5.2 g) in dimethylformamide (10 ml) was added dropwise to a mixture of 50% sodium hydride (1.1 g) and dimethylformamide (20 ml) below 7° C. in 10 minutes and stirred at the same temperature for 30 minutes. Methyl iodide (6.2 g) was added dropwise to the mixture below 7° C. in 15 minutes and stirred at the same temperature for an hour. Chilled water (200 ml) was added to the reaction mixture, and the mixture was extracted with diethyl ether. The extract was washed with water, aqueous sodium hydrogen sulfite and water successively, dried over magnesium sulfate and then evaporated to give oily 2-[2-methoxy-3-(o-tolyloxy)phenyl]-2,2-dimethylacetonitrile (5.7 g).

後処理

  1. stirringstirred at the same temperature for an hour
  2. extractionthe mixture was extracted with diethyl ether
  3. washThe extract was washed with water, aqueous sodium hydrogen sulfite and water successively
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

出典と根拠

ORDレコード
ord-24487fae573c434fba0b5ba7bbb22747
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04367238

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート