Methyl iodide → HCID 53986391、化合物

HRID 440385

反応式

HRID 440385 の反応式
[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]

参加物

9

反応物 4

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

生成物 1

HCID 53986391HCID 53986391、化合物

試薬・触媒・溶媒 4

HCID 887Methanol触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a6bd7bc6093740ba97ec9eedac026529
出典データセット
uspto-grants-1996_05
特許番号
US05519048

関連ノート

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