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

HRID 44256

反応式

HRID 44256 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 23431834Dichloromethane nitromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-00e8b7f346ed4dddbda4d8e0c9474695
出典データセット
uspto-grants-2013_09
特許番号
US08541412B2

関連ノート

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