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Isopropyl iodide → Ethyl 2,6-bis(trifluoromethyl)-4-isopropoxy-5-methyl-3-pyridinecarboxylate

HRID 542131
ノート
印刷プレビュー

反応式

HRID 542131 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([OH:14])[C:6]([CH3:15])=[C:5]([C:16]([F:19])([F:18])[F:17])[N:4]=1.C(=O)([O-])[O-].[K+].[K+].[CH:28](I)([CH3:30])[CH3:29]>CC(C)=O>[F:21][C:2]([F:20])([F:1])[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([O:14][CH:28]([CH3:30])[CH3:29])[C:6]([CH3:15])=[C:5]([C:16]([F:19])([F:18])[F:17])[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 178469144HCID 178469144、化合物

生成物 1

HCID 13882899Ethyl 2,6-bis(trifluoromethyl)-4-isopropoxy-5-methyl-3-pyridinecarboxylate収率 83%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 15.1 g (0.209 mol) of product of Example 35, 6.6 g (0.2 mol) of potassium carbonate, 32 g of isopropyl iodide and 50 ml of acetone was held at reflux for 18 hours and concentrated. The residue was treated with water and filtered. The solid was dissolved in ether (100 ml) and the ether solution was washed with 50 ml of 10% NaOH, dried, and concentrated. The residue was recrystallized from hexane to give 14.2 g (83%) of product; mp 53°-55° C.

後処理

  1. temperatureat reflux for 18 hours
  2. concentrationconcentrated
  3. additionThe residue was treated with water
  4. filtrationfiltered
  5. dissolutionThe solid was dissolved in ether (100 ml)
  6. washthe ether solution was washed with 50 ml of 10% NaOH
  7. customdried
  8. concentrationconcentrated
  9. customThe residue was recrystallized from hexane

出典と根拠

ORDレコード
ord-7fa15f53df234553a9ce781bdd8dd9c3
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04655816

反応ノート

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