Trichloroacetyl chloride → HCID 70922409, 화합물

HRID 524974노트

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HRID 524974 반응식
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](Cl)=[O:4].[CH3:8][C:9]1[CH:13]=[CH:12][NH:11][CH:10]=1>C(OCC)C>[Cl:1][C:2]([Cl:7])([Cl:6])[C:3]([C:12]1[NH:11][CH:10]=[C:9]([CH3:8])[CH:13]=1)=[O:4]

참가 물질

4

반응물 2

HCID 6420Trichloroacetyl chlorideHCID 120231H-Pyrrole, 3-methyl-

생성물 1

HCID 70922409HCID 70922409, 화합물수율 55%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

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온도
45 °C

실험 절차

To a solution of 2,2,2-trichloroacetyl chloride (5.05 mL, 45.3 mmol) in dry diethyl ether (12 mL) was slowly added a solution of 3-methyl-1H-pyrrole (3.15 g, 39.37 mmol) in 30 mL of dry diethyl ether during 1 h 15 min. Once the addition was finished, the reaction mixture was stirred at 45° C. during 1 hour 30 minutes more. Next, more diethyl ether was added and the organic phase was washed with an aqueous solution of potassium carbonate to neutralize de media, water and brine. The organic phase was dried (Na2SO4) and concentrated to dryness to give a residue that was purified by flash chromatography silica (hexane/dichloromethane) to afford 4.7 g of the title compound (55% yield).

후처리

  1. additionOnce the addition
  2. washthe organic phase was washed with an aqueous solution of potassium carbonate
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. concentrationconcentrated to dryness
  5. customto give a residue that
  6. customwas purified by flash chromatography silica (hexane/dichloromethane)

출처 및 근거

ORD 기록
ord-d8226630e89d4b779ad86ddefaff351f
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340547B2

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