Acetone → Ethyl 4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate

HRID 1251952ノート

反応式

HRID 1251952 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[N:5]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14].C([O-])([O-])=O.[K+].[K+].[CH2:24](I)[CH3:25].[CH3:27][C:28](C)=O>>[CH2:27]([O:1][C:2]1[CH:7]=[C:6]([O:8][CH2:24][CH3:25])[N:5]=[C:4]([C:9]([F:12])([F:10])[F:11])[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:28]

参加物

5

反応物 4

HCID 180AcetoneHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 178470040HCID 178470040、化合物

生成物 1

HCID 13726789Ethyl 4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate収率 82.9%

実験手順

This material was prepared in 82.9% yield from product of Example 1 (1 eq), K2CO3 (2 eq) and excess ethyl iodide. The reaction mixture was refluxed in acetone for 18 hours and filtered. The filtrate was concentrated. The residue was dissolved in ether. The ether solution was washed with 10% K2CO3, dried (MgSO4) and concentrated to give the product as an oil, nD25 1.4534.

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated
  3. dissolutionThe residue was dissolved in ether
  4. washThe ether solution was washed with 10% K2CO3
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-efe1bed73b714a7e80930fbb3e47aa1b
出典データセット
uspto-grants-1988_05
特許番号
US04741766

反応ノート

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