Ethylenediamine → 2-Thiophen-2-yl-piperazine

HRID 248478노트

반응식

HRID 248478 반응식
[CH2:1]([NH2:4])[CH2:2][NH2:3].[S:5]1[CH:9]=[CH:8][CH:7]=[C:6]1[C:10](=O)[CH:11]=O.[BH4-].[Na+]>C(O)C>[S:5]1[CH:9]=[CH:8][CH:7]=[C:6]1[CH:10]1[CH2:11][NH:4][CH2:1][CH2:2][NH:3]1

참가 물질

5

반응물 3

HCID 3301EthylenediamineHCID 4311764Sodium borohydrideHCID 52722142-Oxo-2-(thiophen-2-yl)acetaldehyde

생성물 1

HCID 27717262-Thiophen-2-yl-piperazine수율 56.7%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 8.2 g of ethylenediamine in 250 ml of ethanol was added to a solution of 17.64 g of the above aldehyde in 250 ml of ethanol at 0° C. This mixture was stirred at room temperature for 1.5 hours, recooled to 0° C. and 9.6 g of sodium borohydride was added. This mixture was stirred overnight, quenched with water and the ethanol removed. The residue was extracted with dichloromethane, washed with water, dried and evaporated. The residue was crystallized with ether-hexane, giving 12 g of 2-(2-thienyl)piperazine.

후처리

  1. customrecooled to 0° C.
  2. stirringThis mixture was stirred overnight
  3. customquenched with water
  4. customthe ethanol removed
  5. extractionThe residue was extracted with dichloromethane
  6. washwashed with water
  7. customdried
  8. customevaporated
  9. customThe residue was crystallized with ether-hexane

출처 및 근거

ORD 기록
ord-03c5b5351a4a4e46b13c65bdb72b76ca
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210193

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