Methyl iodide → HCID 53986391, 화합물

HRID 440385

반응식

HRID 440385 반응식
[H-].[Na+].[CH:3]([O:5][CH3:6])=[O:4].[F:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15]([O:17][CH3:18])=O)=[CH:10][CH:9]=1.CI>O1CCCC1.CO.CN(C)C=O.O>[CH3:18][O:17][CH:15]=[C:14]([C:11]1[CH:12]=[CH:13][C:8]([F:7])=[CH:9][CH:10]=1)[C:3]([O:5][CH3:6])=[O:4]

참가 물질

9

반응물 4

HCID 6328Methyl iodideHCID 7865Methyl formateHCID 24758Sodium hydrideHCID 2733233Methyl 2-(4-fluorophenyl)acetate

생성물 1

HCID 53986391HCID 53986391, 화합물

시약·촉매·용매 4

HCID 887Methanol촉매HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

Suspend sodium hydride (3.4 g, 142 mmol) in anhydrous tetrahydrofuran (100 mL). Cool in an ice/water bath. Add methyl formate (8.8 mL, 142 mmol), methanol (1 drop), and methyl 4-fluorophenylacetate. Warm slowly to ambient temperature. After 18 hours, concentrate in vacuo to give a residue. Dissolve the residue in dimethylformamide and cool in an ice/water bath. Add methyl iodide (8.0 mL, 130 mmol). Warm slowly to ambient temperature. After 3.5 hours, pour the reaction mixture into water and extract twice with ether. Dry the combined organic layers over MgSO4 filter, and concentrate in vacuo to give the title compound: Rf =0.52 (silica gel, 2/1 hexane/ethyl acetate).

후처리

  1. temperatureCool in an ice/water bath
  2. concentrationconcentrate in vacuo
  3. customto give a residue
  4. temperaturecool in an ice/water bath
  5. temperatureWarm slowly to ambient temperature
  6. waitAfter 3.5 hours
  7. extractionextract twice with ether
  8. dry with materialDry the combined organic layers over MgSO4
  9. filtrationfilter
  10. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-a6bd7bc6093740ba97ec9eedac026529
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05519048

연결된 노트

불러오는 중…