Hydrochloric Acid → (2-Bromo-4-chlorophenyl)methanamine

HRID 2099311

反応式

HRID 2099311 の反応式
[Br:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].Cl.[OH-].[Na+]>C1COCC1>[Br:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 234985242-Bromo-4-chlorobenzonitrile

生成物 1

HCID 57794106(2-Bromo-4-chlorophenyl)methanamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

13.9 ml of borane-THF complex are provided with ice cooling. Slowly a solution of 2.0 g of 2-bromo-4-chlorobenzonitrile (Example 1A) in 60 ml of THF is added. Thereafter the reaction mixture is heated under reflux for 1 h, cooled, and 20 ml of 1N hydrochloric acid are added dropwise, with ice cooling. The mixture is heated under reflux for 1 h and allowed to cool. For the work-up, the solution is rendered alkaline using a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. The crude product is reacted further without purification.

後処理

  1. custom13.9 ml of borane-THF complex are provided with ice cooling
  2. temperatureThereafter the reaction mixture is heated
  3. temperatureunder reflux for 1 h
  4. temperaturecooled
  5. temperatureThe mixture is heated
  6. temperatureunder reflux for 1 h
  7. temperatureto cool
  8. extractionextracted with dichloromethane
  9. dry with materialThe organic phase is dried over sodium sulfate
  10. concentrationconcentrated on a rotary evaporator
  11. customThe crude product is reacted further without purification

出典と根拠

ORDレコード
ord-17fc614e8a3c410eb695b0d8706e5185
出典データセット
uspto-grants-2009_08
特許番号
US07569563B2

関連ノート

読み込み中…