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

HRID 1251951ノート

反応式

HRID 1251951 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+].I[CH:25]([CH3:27])[CH3:26].[CH3:28][C:29]([CH3:31])=O>>[CH:25]([O:1][C:2]1[CH:7]=[C:6]([O:8][CH:29]([CH3:31])[CH3:28])[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])([CH3:27])[CH3:26]

参加物

5

反応物 4

HCID 180AcetoneHCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 178470040HCID 178470040、化合物

生成物 1

HCID 13726788Ethyl 4,6-diisopropoxy-2-(trifluoromethyl)-3-pyridinecarboxylate収率 98%

実験手順

A mixture of 37.3 g of product of Example 1, 41 g of potassium carbonate, 99 g of 2-iodopropane and 300 ml of acetone was held at reflux for 21 hours. The reaction mixture was filtered. The acetone filtrate was concentrated. The residue was taken into ether and the ether solution was washed with 10% sodium hydroxide, dried, and concentrated. The residue was kugelrohr distilled to give 48.8 g (98%) of product, nD25 1.4491.

後処理

  1. temperatureat reflux for 21 hours
  2. filtrationThe reaction mixture was filtered
  3. concentrationThe acetone filtrate was concentrated
  4. washthe ether solution was washed with 10% sodium hydroxide
  5. customdried
  6. concentrationconcentrated
  7. distillationThe residue was kugelrohr distilled

出典と根拠

ORDレコード
ord-da863c1feb624a07a9c7094d305ea8db
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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