Ammonia → 5-(3,4-Dibromobutyl)pyridine-2-carboxamide

HRID 1580972

反応式

HRID 1580972 の反応式
[Br:1][CH:2]([CH2:14][Br:15])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11](O)=[O:12])=[N:9][CH:10]=1.S(Cl)(Cl)=O.[NH3:20]>C(Cl)(Cl)Cl>[Br:1][CH:2]([CH2:14][Br:15])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]([NH2:20])=[O:12])=[N:9][CH:10]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 24386Thionyl ChlorideHCID 2167205-(3,4-Dibromobutyl)pyridine-2-carboxylic acid

生成物 1

HCID 132718775-(3,4-Dibromobutyl)pyridine-2-carboxamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
50 °C

実験手順

20 g of 5-(3,4-dibromobutyl)picolinic acid was added to 15 ml of thionyl chloride and resulting solution was kept to warm at 50°C for one-half hour. Reaction mixture was evaporated in reduced pressure and resulting oily residue was dissolved in chloroform 100 ml. Through the solution dry ammonia gas was passed for five minutes with cooling. White precipitate was removed by filtration and washed with chloroform. Filtrate and washings are combined and evaporated in reduced pressure. Resulting solid was crystallized from benzene to give 10.2 g of the pure product as platelets.

後処理

  1. customresulting solution
  2. customReaction mixture
  3. customwas evaporated in reduced pressure
  4. customresulting oily residue
  5. temperaturewith cooling
  6. customWhite precipitate was removed by filtration
  7. washwashed with chloroform
  8. customevaporated in reduced pressure
  9. customResulting solid
  10. customwas crystallized from benzene

出典と根拠

ORDレコード
ord-024697468ebd42488821dcb604921c7d
出典データセット
uspto-grants-1976_01
特許番号
US03935221

関連ノート

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