Hydrochloric Acid → 3,4-Dibenzyloxyphenylacetonitrile

HRID 1440375노트

반응식

HRID 1440375 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 109097272-(3,4-Dihydroxyphenyl)acetonitrile

생성물 1

HCID 27580313,4-Dibenzyloxyphenylacetonitrile

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d41e603b53c4fa391571d38ccf8ec84
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05498746

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