Hydrochloric Acid → HCID 178478463、化合物

HRID 863739

反応式

HRID 863739 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]#[N:7].[N-:8]=[N+:9]=[N-:10].[Na+].[Cl-].[Al+3].[Cl-].[Cl-].Cl>O1CCCC1.CCCCC>[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[NH:10][N:9]=[N:8][N:7]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 804745-ChlorovaleronitrileHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 178478463HCID 178478463、化合物

試薬・触媒・溶媒 2

HCID 8003Pentane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

100mmol of 5-chlorovaleronitrile are placed under an inert atmosphere in 100 ml of anhydrous tetrahydrofuran on an ice bath. 445 mmol of sodium azide and then 100 mmol of aluminum chloride are then added in small fractions. The reaction mixture is heated to 80° C. and left under reflux, with stirring, for 16 hours. The complex formed is then hydrolyzed by addition, dropwise, of 150 cm3 of 5% hydrochloric acid. The resulting aqueous phase is extracted with ethyl acetate and after washing the organic phase with water, then with a saturated sodium chloride solution, drying and evaporation, the residue obtained is taken up in pentane. The expected product is then obtained after filtration of the precipitate formed.

後処理

  1. waitleft
  2. temperatureunder reflux
  3. customThe complex formed
  4. additionis then hydrolyzed by addition
  5. extractionThe resulting aqueous phase is extracted with ethyl acetate
  6. washafter washing the organic phase with water
  7. dry with materialwith a saturated sodium chloride solution, drying
  8. customevaporation
  9. customthe residue obtained

出典と根拠

ORDレコード
ord-7c5079c0fe654c1b83febdf8eee3497c
出典データセット
uspto-grants-1996_10
特許番号
US05561113

関連ノート

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