Hydrochloric Acid → 3,4-Dibenzyloxyphenylacetonitrile

HRID 1440375ノート

反応式

HRID 1440375 の反応式
[OH:1][C:2]1[C:7](O)=[CH:6][C:5]([CH2:9][C:10]#[N:11])=[CH:4][CH:3]=1.[C:12](=[O:15])([O-])[O-].[K+].[K+].[CH2:18](Cl)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.Cl>CN(C)C=O.O>[CH2:18]([O:1][C:2]1[C:7]([O:15][CH2:12][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:6][C:5]([CH2:9][C:10]#[N:11])=[CH:4][CH:3]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

7

実験手順

A mixture consisting of one mole (149 g) of 4,5-dihydroxyphenylacetonitrile prepared in stage 1, two moles of potassium carbonate (276 g) and 2.2 moles (278.5 g) of benzyl chloride in 745 ml of dimethylformamide is heated to 105°-110° C. for approximately 30 minutes. At the end of the reaction, the reaction mixture is diluted with 2.5 kg of a mixture of ice and water, and is neutralized with hydrochloric acid while being briskly stirred. The expected product, which has precipitated, is filtered off, washed with water, and is again mixed into a paste with ethanol and then with isopropyl:ether.

後処理

  1. temperatureis heated to 105°-110° C. for approximately 30 minutes
  2. customAt the end of the reaction
  3. customThe expected product, which has precipitated
  4. filtrationis filtered off
  5. washwashed with water
  6. additionis again mixed into a paste with ethanol

出典と根拠

ORDレコード
ord-5d41e603b53c4fa391571d38ccf8ec84
出典データセット
uspto-grants-1996_03
特許番号
US05498746

反応ノート

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