Methyl iodide → HCID 58265699, 화합물

HRID 1874079노트

반응식

HRID 1874079 반응식
[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]

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 24758Sodium hydrideHCID 2746295N-(4-Bromo-3-chlorophenyl)acetamide

생성물 1

HCID 58265699HCID 58265699, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-81812a8da37240fcbe1a04f9cf70e2a2
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304556B2

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