Hydrochloric Acid → HCID 86753552、化合物

HRID 342423

反応式

HRID 342423 の反応式
[CH3:1][C:2]1[O:6][C:5]2[C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=[CH:10][C:4]=2[CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[CH3:18][O:19]C(Cl)Cl.Cl>ClCCl>[CH:18]([C:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:5]=2[O:6][C:2]=1[CH3:1])=[O:19]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 21004Methane, dichloromethoxy-HCID 6451240Aluminum(III) ChlorideHCID 132018972-Methyl-7-nitrobenzofuran

生成物 1

HCID 86753552HCID 86753552、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a mixture of 2-methyl-7-nitrobenzo[b]furan (1.77 g) and aluminum chloride (2.66 g) in dichloromethane (40 ml) was added dropwise a solution of dichloromethyl methyl ether (3.6 ml) in dichloromethane (10 ml). The mixture was stirred at ambient temperature for 30 minutes and the reaction mixture was poured into a mixture of ice and 1N-hydrochloric acid. The separated oil was extracted with dichloromethane and the extract was washed with brine, aqueous saturated sodium bicarbonate and brine. Then, the solution was dried over sodium sulfate and evaporated in vacuo. The obtained oil was crystallized from diethyl ether to give 3-formyl-2-methyl-7-nitrobenzo[b]furan (1.83 g).

後処理

  1. extractionThe separated oil was extracted with dichloromethane
  2. washthe extract was washed with brine, aqueous saturated sodium bicarbonate and brine
  3. dry with materialThen, the solution was dried over sodium sulfate
  4. customevaporated in vacuo
  5. customThe obtained oil was crystallized from diethyl ether

出典と根拠

ORDレコード
ord-02a255bdb6784c9caf126c55bafac015
出典データセット
uspto-grants-1999_01
特許番号
US05858995

関連ノート

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