Methyl iodide → HCID 58265699、化合物

HRID 1874079ノート

反応式

HRID 1874079 の反応式
[CH3:1][C:2]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([Br:11])=[C:7]([Cl:12])[CH:6]=1)=[O:3].[H-].[Na+].[CH3:15]I>C1COCC1>[Br:11][C:8]1[CH:9]=[CH:10][C:5]([N:4]([CH3:15])[C:2](=[O:3])[CH3:1])=[CH:6][C:7]=1[Cl:12]

参加物

5

反応物 3

HCID 6328Methyl iodide2 回HCID 24758Sodium hydrideHCID 2746295N-(4-Bromo-3-chlorophenyl)acetamide

生成物 1

HCID 58265699HCID 58265699、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-bromo-3-chloroacetanilide (10.0 g, 40.2 mmol) in 50 mL THF is added 60% sodium hydride in mineral oil (2.40 g, 60.0 mmol) and the reaction mixture is stirred for 1 h at RT. The reaction mixture is cooled to 0° C., methyliodide (2.49 mL, 40.0 mmol) is added. After 2 h additional methyl iodide (0.25 mL, 4.0 mmol) is added and the reaction mixture is stirred at RT for 10 min. The reaction mixture is quenched with saturated aqueous ammonium chloride, filtered and extracted with diethyl ether. The organic phases are washed with brine, dried over Na2SO4 and evaporated to dryness. Yield: 10.3 g.

後処理

  1. temperatureThe reaction mixture is cooled to 0° C.
  2. stirringthe reaction mixture is stirred at RT for 10 min
  3. customThe reaction mixture is quenched with saturated aqueous ammonium chloride
  4. filtrationfiltered
  5. extractionextracted with diethyl ether
  6. washThe organic phases are washed with brine
  7. dry with materialdried over Na2SO4
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-81812a8da37240fcbe1a04f9cf70e2a2
出典データセット
uspto-grants-2012_11
特許番号
US08304556B2

反応ノート

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