Water → 3-Bromo-2-(2,2,2-trifluoroethoxy)-5-(trifluoromethyl)pyridine

HRID 1976061ノート

反応式

HRID 1976061 の反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].[Br:9][C:10]1[C:11](Cl)=[N:12][CH:13]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:15]=1.O>O1CCCC1>[Br:9][C:10]1[C:11]([O:4][CH2:3][C:2]([F:6])([F:5])[F:1])=[N:12][CH:13]=[C:14]([C:16]([F:18])([F:17])[F:19])[CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 135360613-Bromo-2-chloro-5-(trifluoromethyl)pyridine

生成物 1

HCID 220002003-Bromo-2-(2,2,2-trifluoroethoxy)-5-(trifluoromethyl)pyridine収率 62.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 2,2,2-trifluoroethanol (1.4 mL, 19.2 mmol) in tetrahydrofuran (3 mL) was added sodium hydride (60% suspension in oil, 760 mg, 19.0 mmol) and the suspension formed was stirred for 20 minutes. 3-Bromo-2-chloro-5-trifluoromethylpyridine (1.0 g, 3.84 mmol) was then added and the solution stirred at room temperature for 16 hrs. Water (100 mL) was added and the mixture formed was extracted with ethyl acetate (2×100 mL). The extracts were dried (MgSO4) and concentrated to give the product as an oil (776 mg, 2.4 mmol, 62% yield).

後処理

  1. customthe suspension formed
  2. stirringthe solution stirred at room temperature for 16 hrs
  3. customthe mixture formed
  4. extractionwas extracted with ethyl acetate (2×100 mL)
  5. dry with materialThe extracts were dried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-28913db90a0d4f64a818599b0b9536e3
出典データセット
uspto-grants-2001_05
特許番号
US06225320B1

反応ノート

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