Ethylenediamine → 2-Thiophen-2-yl-piperazine

HRID 248478ノート

反応式

HRID 248478 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 27717262-Thiophen-2-yl-piperazine収率 56.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03c5b5351a4a4e46b13c65bdb72b76ca
出典データセット
uspto-grants-1993_05
特許番号
US05210193

反応ノート

読み込み中…