Borane;tetrahydrofuran → N-(2-methylaminoethyl)homopiperazine

HRID 1288828ノート

反応式

HRID 1288828 の反応式
[CH:1]([NH:3][CH2:4][CH2:5][N:6]1[CH2:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=O.B.C1COCC1>C1COCC1>[CH3:1][NH:3][CH2:4][CH2:5][N:6]1[CH2:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1

参加物

4

反応物 2

HCID 2723981Borane;tetrahydrofuranHCID 18924841HCID 18924841、化合物

生成物 1

HCID 18924839N-(2-methylaminoethyl)homopiperazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2.75 gm of N-(2-formamidoethyl)homopiperazine in 20 ml of dry THF under N2 is added carefully 60 ml of borane THF solution. After the addition is complete the reaction mixture is heated to reflux for 5 hours then stirred at room temperature overnight. The reaction mixture is quenched by the careful addition of 20 ml of 6N HCl followed by refluxing for 1 hour. The reaction mixture is cooled, 50 ml of water added and solid KOH added carefully to alkaline pH. Extraction with ether gives the desired product N-(2-methylamino)homopiperazine.

後処理

  1. additionAfter the addition
  2. temperatureis heated
  3. temperatureto reflux for 5 hours
  4. customThe reaction mixture is quenched by the careful addition of 20 ml of 6N HCl
  5. temperatureby refluxing for 1 hour
  6. temperatureThe reaction mixture is cooled
  7. addition50 ml of water added
  8. additionsolid KOH added carefully
  9. extractionExtraction with ether

出典と根拠

ORDレコード
ord-621ac7fd636f4d7f90a5c09791ef57b4
出典データセット
uspto-grants-1998_05
特許番号
US05747485

反応ノート

読み込み中…