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

HRID 1976061노트

반응식

HRID 1976061 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-28913db90a0d4f64a818599b0b9536e3
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225320B1

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