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2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine → 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine

HRID 366299
笔记
打印预览

反应方程式

HRID 366299 反应方程式
C[O-].[K+].[CH3:4][N:5]1[C:9]([O:10][C:11]2[CH:16]=[C:15]([O:17][C:18]3N(C)N=C(C(F)(F)F)C=3)[CH:14]=[C:13]([O:28][C:29]3[N:33]([CH3:34])[N:32]=[C:31]([C:35]([F:38])([F:37])[F:36])[CH:30]=3)[N:12]=2)=[CH:8][C:7]([C:39]([F:42])([F:41])[F:40])=[N:6]1>CO>[CH3:34][N:33]1[C:29]([O:28][C:13]2[CH:14]=[C:15]([O:17][CH3:18])[CH:16]=[C:11]([O:10][C:9]3[N:5]([CH3:4])[N:6]=[C:7]([C:39]([F:40])([F:41])[F:42])[CH:8]=3)[N:12]=2)=[CH:30][C:31]([C:35]([F:38])([F:36])[F:37])=[N:32]1
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 158696782,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridineHCID 23664618甲醇钾

产物 1

HCID 225726302,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine收率 43.4%

试剂、催化剂与溶剂 1

HCID 887Methanol溶剂2 次

实验过程

A 3 ml aliquot of a 25 % solution of potassium methylate (10 mmol) in dry methanol is added to a solution of 5.7 g (10 mmol) 2,4,6-tris-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine in 20 ml anhydrous methanol. After 2 hours at ambient temperature, the reaction mixture is heated to reflux. The solvent is removed under reduced pressure and ethyl acetate is added to the residue. The mixture is washed with a 2 N sodium hydroxide solution. After drying and filtration of the organic layer, the solvents are removed and the residue is washed with diisopropyl ether and pentane. Colorless crystals (1.9 g, 43 % yield) of melting point 107° C. are obtained.

后处理

  1. temperaturethe reaction mixture is heated to reflux
  2. customThe solvent is removed under reduced pressure and ethyl acetate
  3. additionis added to the residue
  4. washThe mixture is washed with a 2 N sodium hydroxide solution
  5. customAfter drying
  6. filtrationfiltration of the organic layer
  7. customthe solvents are removed
  8. washthe residue is washed with diisopropyl ether and pentane

来源与证据

ORD记录
ord-6759362e203b434a933ffc01546fab73
来源数据集
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06130188

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