Dimethylformamide → 4-(2,2,2-Trifluoro-1-methyl-1-(trifluoromethyl)ethyl)anisole

HRID 1634353노트

반응식

HRID 1634353 반응식
[F:1][C:2]([F:16])=[C:3]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)[C:4]([F:7])([F:6])[F:5].CI.[F-:19].[Cs+].[CH3:21]N(C=O)C>O>[F:19][C:2]([F:16])([F:1])[C:3]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)([CH3:21])[C:4]([F:5])([F:6])[F:7]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 25953Cesium fluorideHCID 117763304-(2,2-Difluoro-1-(trifluoromethyl)ethenyl)anisole

생성물 1

HCID 186776014-(2,2,2-Trifluoro-1-methyl-1-(trifluoromethyl)ethyl)anisole수율 10%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

A mixture of Compound 74 (570 mg, 2.4 mmol), MeI (430 mg, 3.0 mmol), and CsF (760 mg, 5.0 mmol) in DMF (4 ml) was stirred at 80° C. for 3 days. The mixture was diluted with H2O. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined solution was dried (Na2SO4) and concentrated in vacuo to give crude product, which was purified by column chromatography on silica gel to give Compound 75 (70 mg, 10%) as a yellow oil.

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with CH2Cl2
  3. dry with materialThe combined solution was dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customto give crude product, which
  6. customwas purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-665f97d163074b4a8d115c57072eb292
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06506775B1

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