三乙胺 → 2-羟基喹啉-4-羧酸甲酯

HRID 6811

反应方程式

HRID 6811 反应方程式
I[C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].C/[C:10](/[C:16]([O-:18])=[O:17])=[C:11](\C)/[C:12]([O-:14])=O.[CH2:19](N(CC)CC)C>C([O-])(=O)C.C([O-])(=O)C.[Pd+2].C(#N)C>[O:14]=[C:12]1[CH:11]=[C:10]([C:16]([O:18][CH3:19])=[O:17])[C:2]2[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=2)[NH:4]1

参与物

6

反应物 3

HCID 8471三乙胺HCID 119952-碘苯胺HCID 5459894Dimethylmaleate

产物 1

HCID 1816362-羟基喹啉-4-羧酸甲酯

试剂、催化剂与溶剂 2

HCID 167845palladium acetate催化剂HCID 6342乙腈溶剂

实验过程

In a heavy-walled PYREX tube was placed 2-iodoaniline (2.84 g, 13 mmol), dimethylmaleate (2.44 g, 17 mmol), triethylamine (1.4 mL, 10 mmol), palladium diacetate (31 mg, 0.14 mmol) and 6 mL acetonitrile. The tube was flushed with nitrogen and sealed. The sealed tube was heated at 100° for 3.5 h then cooled to r.t. The tube was opened and the resulting solids filtered and washed with acetonitrile. The solids were dissolved in chloroform and the solvent removed under vacuum to provide a solid.

后处理

  1. customThe tube was flushed with nitrogen
  2. customsealed
  3. temperatureThe sealed tube was heated at 100° for 3.5 h
  4. filtrationthe resulting solids filtered
  5. washwashed with acetonitrile
  6. dissolutionThe solids were dissolved in chloroform
  7. customthe solvent removed under vacuum
  8. customto provide a solid

来源与证据

ORD记录
ord-ce024ddd171d42738801fd911c4752bb
来源数据集
uspto-grants-2006_08
专利号
US07084156B2

关联笔记

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