Acetic Acid → 4-Cyanobenzyl acetate

HRID 635537노트

반응식

HRID 635537 반응식
[C:1]([C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][CH:4]=1)#N.O.C(Cl)Cl.N([O-])=O.[Na+].[C:19]([OH:22])(=[O:21])[CH3:20]>>[C:19]([O:22][CH2:1][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1)(=[O:21])[CH3:20]

참가 물질

6

반응물 5

HCID 176Acetic AcidHCID 962WaterHCID 6344DichloromethaneHCID 826084-(Aminomethyl)benzonitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 114466294-Cyanobenzyl acetate수율 84%

실험 절차

p-Cyanobenzylamine (13.2 g), water (18 g), and methylene chloride (18 g) were mixed, and the mixture was stirred with cooling with ice. Acetic acid (18 g) was added to the mixture. Subsequently, a 20 wt % aqueous solution (51.8 g) of sodium nitrite was added dropwise to the mixture over a one hour period. The mixture was stirred at the same temperature for four hours. The reaction mixture was subjected to extraction with methylene chloride, and the organic solvent was concentrated. Water was added to the concentrated solution, and the residual organic solvent was removed through distillation, to thereby obtain 14.7 g of p-cyanobenzyl acetate (yield 84%). The purity of the product was 98%.

후처리

  1. temperaturewith cooling with ice
  2. stirringThe mixture was stirred at the same temperature for four hours
  3. extractionThe reaction mixture was subjected to extraction with methylene chloride
  4. concentrationthe organic solvent was concentrated
  5. additionWater was added to the concentrated solution
  6. customthe residual organic solvent was removed through distillation

출처 및 근거

ORD 기록
ord-e8120d1702624887becbb79e6cdab7f8
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06187945B1

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