聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 吡咯并[1,2-B]哒嗪-4(1H)-酮

HRID 347472笔记

反应方程式

HRID 347472 反应方程式
[O:1]=[C:2]1[C:7](C(OCC)=O)=[CH:6][NH:5][N:4]2[CH:13]=[CH:14][CH:15]=[C:3]12.[Na+].[Cl-].O>CS(C)=O>[NH:5]1[CH:6]=[CH:7][C:2](=[O:1])[C:3]2=[CH:15][CH:14]=[CH:13][N:4]12

参与物

5

反应物 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 5234Halite (NaCl)HCID 101044214-氧代-1,4-二氢吡咯并[1,2-B]哒嗪-3-甲酸乙酯

产物 1

HCID 57415871吡咯并[1,2-B]哒嗪-4(1H)-酮收率 67.1%

试剂、催化剂与溶剂 1

HCID 679二甲基亚砜溶剂2 次

反应条件

温度
150 °C

实验过程

A mixture of ethyl 4-oxo-1,4-dihydropyrrolo[1,2-b]pyridazine-3-carboxylate (206 mg, 1.0 mmol), NaCl (64 mg, 1.1 mmol), water (0.054 mL, 3.0 mmol) and DMSO (2 mL) was heated at 150° C. for 3 hours. At the end of the reaction DMSO was distilled off and the residue was purified by silica gel flash chromatography (eluted with 1–10% EtOAc/CH2Cl2) to give the title compound (90 mg, 67%) as a light yellow solid.

后处理

  1. distillationwas distilled off
  2. customthe residue was purified by silica gel flash chromatography (eluted with 1–10% EtOAc/CH2Cl2)

来源与证据

ORD记录
ord-b3551cdbfd064d4ba62240ba41e1392c
来源数据集
uspto-grants-2007_02
专利号
US07173031B2

反应笔记

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