Sodium Iodide → 2,3-Dicyanonaphthalene

HRID 1090288

反応式

HRID 1090288 の反応式
Br[C:2]1[C:3](Br)=[C:4](Br)[C:5](Br)=[C:6]([CH3:9])[C:7]=1[CH3:8].[C:13](#[N:18])/[CH:14]=[CH:15]/[C:16]#[N:17].[I-].[Na+].S([O-])(O)=O.[Na+]>CN(C)C=O>[C:16]([C:15]1[C:14]([C:13]#[N:18])=[CH:8][C:7]2[C:6](=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:9]=1)#[N:17]

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 177713,4,5,6-Tetrabromo-o-xyleneHCID 637930FumaronitrileHCID 23665763Sodium Bisulfite

生成物 1

HCID 6012702,3-Dicyanonaphthalene収率 80%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

To 0.1 mole of tetrabromoxylene, 0.17 mole of fumaronitrile, 0.66 mole of sodium iodide and 400 ml of anhydrous dimethylformamide were added and heated with stirring at 70 to 80° C. for 7 hours. The reaction solution was added to 800 g of ice water. To the deposited precipitate, about 15 g of sodium hydrogen sulfite was added and allowed to stand overnight. After filtration by suction and drying, while 2,3-dicyanonaphthalene was obtained by recrystallization from chloroform/ethanol in yield of 80%.

後処理

  1. temperatureheated
  2. waitto stand overnight
  3. filtrationAfter filtration by suction
  4. dry with materialdrying, while 2,3-dicyanonaphthalene
  5. customwas obtained by recrystallization from chloroform/ethanol in yield of 80%

出典と根拠

ORDレコード
ord-9055e085ce8c43f884016c9c975cd909
出典データセット
uspto-grants-1992_01
特許番号
US05081236

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