Methyl iodide → HCID 66859027, 화합물

HRID 1803152노트

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HRID 1803152 반응식
[H-].[Na+].[F:3][C:4]1[C:9]([F:10])=[CH:8][C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:5]=1[OH:14].I[CH3:16]>CN(C=O)C.C1COCC1>[F:10][C:9]1[CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=[C:5]([O:14][CH3:16])[C:4]=1[F:3]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 221546562,3-Difluoro-5-nitrophenol

생성물 1

HCID 66859027HCID 66859027, 화합물수율 49.1%

시약·촉매·용매 1

HCID 21974620tetrahydrofuran N,N-dimethylformamide용매

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온도
80 °C

실험 절차

Step M (4): Sodium hydride (120 mg, 5 mmol) was added to a solution of 2,3-difluoro-5-nitrophenol (250 mg, 1.4 mmol) in DMF/THF (4 mL/4 mL). After 10 min, iodomethane (0.2 mL, 5 mmol) was added. The mixture was heated at 80° C. for 2 h. The reaction mixture was quenched with 1 N HCl. The mixture was diluted with water and extracted with EtOAc. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford 1,2-difluoro-3-methoxy-5-nitrobenzene (130 mg, 48% yield).

후처리

  1. customThe reaction mixture was quenched with 1 N HCl
  2. additionThe mixture was diluted with water
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-114c7bea4d444778843b552a07b23c9c
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349880B2

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