Methane, dichloromethoxy- → 5-Trichloroacetyl-1H-pyrrole-3-carbaldehyde

HRID 44256

반응식

HRID 44256 반응식
[Cl:1][C:2]([Cl:11])([Cl:10])[C:3]([C:5]1[NH:6][CH:7]=[CH:8][CH:9]=1)=[O:4].[Al+3].[Cl-].[Cl-].[Cl-].Cl[CH:17](Cl)[O:18]C>C(Cl)Cl.[N+](C)([O-])=O>[Cl:11][C:2]([Cl:1])([Cl:10])[C:3]([C:5]1[NH:6][CH:7]=[C:8]([CH:17]=[O:18])[CH:9]=1)=[O:4]

참가 물질

5

반응물 3

HCID 21004Methane, dichloromethoxy-HCID 3214872-(Trichloroacetyl)pyrroleHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 124599775-Trichloroacetyl-1H-pyrrole-3-carbaldehyde

시약·촉매·용매 1

HCID 23431834Dichloromethane nitromethane용매

실험 절차

To a solution of the compound obtained in Step A (87 mmoles) and AlCl3 in a DCM/nitromethane mixture (80 ml/80 ml) there is added, dropwise, at −30° C., dichloro-methoxy-methane (130.5 mmoles). After stirring for two hours, the reaction mixture is poured into 800 ml of ice-cold water. The aqueous phase is extracted with AcOEt, and then the organic phases are combined. The organic phase is washed with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product (brown crystals), which is used directly in the next Step.

후처리

  1. customat −30° C.
  2. extractionThe aqueous phase is extracted with AcOEt
  3. washThe organic phase is washed with saturated aqueous NaCl solution
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-00e8b7f346ed4dddbda4d8e0c9474695
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541412B2

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