1-(2-Hydroxyethyl)piperazine → HCID 22272590, 화합물

HRID 1064817노트

반응식

HRID 1064817 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:17][C:18]#[N:19]>C(#N)C>[C:18]([CH2:17][N:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][OH:1])[CH2:5][CH2:6]1)#[N:19]

참가 물질

5

반응물 3

HCID 76771-(2-Hydroxyethyl)piperazineHCID 7856ChloroacetonitrileHCID 11430Potassium Carbonate

생성물 1

HCID 22272590HCID 22272590, 화합물수율 95%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 1-(2-hydroxyethyl)piperazine (2.60 g, 20 mmol) in acetonitrile (35 ml) was added potassium carbonate (3.04 g, 22 mmol) and chloroacetonitrile (1.51 g, 20 mmol) was dropped thereinto with ice cooling. The mixture was stirred at room temperature for 30 minutes and then stirred at 45° C. for 30 minutes. This reaction mixture was filtered off, the filtrate was concentrated in vacuo and the residue was purified by a silica gel column chromatography (100 g of silica gel; developing solvent, chloroform:ammonia-saturated methanol=20:1→10:1) to provide 3.20 g (yield 95%) of 4-(cyanomethyl)piperazine-1-ethanol.

후처리

  1. additionwas dropped
  2. stirringstirred at 45° C. for 30 minutes
  3. filtrationThis reaction mixture was filtered off
  4. concentrationthe filtrate was concentrated in vacuo
  5. customthe residue was purified by a silica gel column chromatography (100 g of silica gel; developing solvent, chloroform:ammonia-saturated methanol=20:1→10:1)

출처 및 근거

ORD 기록
ord-936ecfab76e64f38a98714768ecd7c58
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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