Acetic Anhydride → 3-Tolunitrile

HRID 651294노트

반응식

HRID 651294 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=[O:3])[CH3:2].[Br-].[NH4+].[C:10]([C:12]1[CH:13]=[C:14]([CH3:18])[CH:15]=[CH:16][CH:17]=1)#[N:11].O.[C:20](O)(=[O:22])[CH3:21]>C([O-])(=O)C.[Zn+2].C([O-])(=O)C>[C:10]([C:12]1[CH:13]=[C:14]([CH3:18])[CH:15]=[CH:16][CH:17]=1)#[N:11].[C:1]([O:4][CH:5]([O:7][C:20](=[O:22])[CH3:21])[C:6]1[CH:15]=[CH:16][CH:17]=[C:12]([C:10]#[N:11])[CH:13]=1)(=[O:3])[CH3:2]

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 121043-TolunitrileHCID 25514Ammonium Bromide2회HCID 21899381Acetic acid--water (1/1)

생성물 2

HCID 121043-TolunitrileHCID 53968160m-Cyanobenzylidene diacetate

시약·촉매·용매 1

HCID 11192Zinc Acetate촉매

실험 절차

A glass three-neck flask was charged with 106.3 g of acetic anhydride, 0.67 g of cerous (III) acetate monohydrate, 0.88 g of zinc (II) acetate dehydrate and 0.78 g of ammonium bromide, and the mixture was stirred at 500 rpm using stirring blades, while air was bubled in at 150 ml/min at atmospheric pressure. In succession, the three-neck flask was heated in an oil back, to be kept at 90° C., and 14.9 g of m-cyanotoluene was added at a time from a dropping funnel, to start reaction. After initiation of reaction, 0.1 g of ammonium bromide was added every hour 8 times. The reaction solution was sampled at predetermined time intervals and analyzed by high performance liquid chromatography. The m-cyanotoluene conversion and m-cyanobenzylidene diacetate yield were calculated from the following formulae:

후처리

  1. stirringusing stirring blades
  2. temperatureIn succession, the three-neck flask was heated in an oil back
  3. customto be kept at 90° C.
  4. customreaction
  5. additionwas added every hour 8 times
  6. aliquotThe reaction solution was sampled at predetermined time intervals

출처 및 근거

ORD 기록
ord-4014d31ecae94e85a659d2d5b6cb4dca
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06278019B1

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