Sodium Iodide → 2,3-Dicyanonaphthalene

HRID 476831

反応式

HRID 476831 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 mol of tetrabromoxylene were added 0.17 mol of fumaronitrile, 0.66 mol of sodium iodide and 400 ml of anhydrous dimethylformamide, and the mixture was stirred under heating at 70° to 80° C. for 7 hours. The reaction mixture was added to 800 g of ice-water, and to the resultant precipitate was added about 15 g of sodium hydrogen sulfite and the mixture was left to stand overnight. Subsequently, the mixture was filtered and dried, followed by recrystallization from chloroform/ethanol, to give white 2,3-dicyanonaphthalene. The yield was 80%.

後処理

  1. temperatureunder heating at 70° to 80° C. for 7 hours
  2. waitthe mixture was left
  3. filtrationSubsequently, the mixture was filtered
  4. customdried
  5. customfollowed by recrystallization from chloroform/ethanol

出典と根拠

ORDレコード
ord-1eb695f3a2a048318e8379ef2fd4ce61
出典データセット
uspto-grants-1989_12
特許番号
US04886721

関連ノート

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