Acetic Anhydride → 3-Tolunitrile

HRID 651294

反応式

HRID 651294 の反応式
[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]

参加物

7

反応物 4

HCID 7918Acetic AnhydrideHCID 121043-TolunitrileHCID 25514Ammonium Bromide2 回HCID 21899381Acetic acid--water (1/1)

生成物 2

HCID 121043-TolunitrileHCID 53968160m-Cyanobenzylidene diacetate

試薬・触媒・溶媒 1

HCID 11192Zinc Acetate触媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-4014d31ecae94e85a659d2d5b6cb4dca
出典データセット
uspto-grants-2001_08
特許番号
US06278019B1

関連ノート

読み込み中…