Sodium Iodide → 2,3-Dicyanonaphthalene

HRID 22458

反応式

HRID 22458 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

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, white 2,3-dicyano-naphthalene 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. customdrying

出典と根拠

ORDレコード
ord-72aec833b8cf48679a26494ee945d873
出典データセット
uspto-grants-1995_06
特許番号
US05428152

関連ノート

読み込み中…