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

HRID 1288828노트

반응식

HRID 1288828 반응식
[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

참가 물질

4

반응물 2

HCID 2723981Borane;tetrahydrofuranHCID 18924841HCID 18924841, 화합물

생성물 1

HCID 18924839N-(2-methylaminoethyl)homopiperazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-621ac7fd636f4d7f90a5c09791ef57b4
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05747485

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