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乙醇 → 2-[4-(4-Pyridinyl)piperazino]ethylamine

HRID 1663229
笔记
打印预览

反应方程式

HRID 1663229 反应方程式
[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][N:15]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:9][CH2:8]2)=[CH:3][CH:2]=1.C(O)C.O.O.NN>C(OCC)C>[N:1]1[CH:2]=[CH:3][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][NH2:15])[CH2:9][CH2:8]2)=[CH:5][CH:6]=1
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 702乙醇HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 24654水合肼HCID 674365642-[2-(4-Pyridin-4-yl-piperazin-1-yl)-ethyl]-isoindole-1,3-dione

产物 1

HCID 184406752-[4-(4-Pyridinyl)piperazino]ethylamine收率 62.2%

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

实验过程

A stirred mixture of 2-[2-(4-pyridin-4-yl-piperazin-1-yl)-ethyl]-isoindole-1,3-dione (1.52 g, 4.52 mmol), ethanol (47.5 mL), water (2.5 mL) and hydrazine hydrate (98%, 0.438 mL, 9.04 mmol) was refluxed for 3 h, then cooled and diluted with diethyl ether (100 mL). The precipitated crystals were filtered off, washed with diethyl ether and filtrate was concentrated. The residue was dissolved N sodium hydroxide (25 mL), extracted with dichloromethane (4×25 mL), the combined organic layers were washed with brine (25 mL), dried over sodium sulfate, filtered and concentrated to yield 0.58 g (62%) of the title compound as a colorless oil.

后处理

  1. temperaturewas refluxed for 3 h
  2. temperaturecooled
  3. filtrationThe precipitated crystals were filtered off
  4. washwashed with diethyl ether and filtrate
  5. concentrationwas concentrated
  6. dissolutionThe residue was dissolved N sodium hydroxide (25 mL)
  7. extractionextracted with dichloromethane (4×25 mL)
  8. washthe combined organic layers were washed with brine (25 mL)
  9. dry with materialdried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated

来源与证据

ORD记录
ord-55f9490a13a146e2a0594283cc5b6c7b
来源数据集
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08034827B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记