4,4'-Dimethoxybenzophenone → Bis(4-methoxyphenyl)diazomethane

HRID 1278159ノート

反応式

HRID 1278159 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)=O)=[CH:5][CH:4]=1.[NH2:19][NH2:20]>C(O)CC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)=[N+:19]=[N-:20])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 70324,4'-DimethoxybenzophenoneHCID 9321Hydrazine

生成物 1

HCID 4544348Bis(4-methoxyphenyl)diazomethane

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

25 grams (0.1 moles) of p,p'-dimethoxybenzophenone, which was purchased from the Aldrich Chemical Company, was dissolved in 50 ml of n-propanol and with solution was treated with 20 grams of hydrazine, which had been freshly distilled over sodium hydroxide pellets. The mixture was then refluxed for a total of 12 hours, after which the solvent (n-propanol) and excess hydrozine were removed at reduced pressure. The residual crude hydrazone was recrystallized from ethanol and had a melting point of 85° C.

後処理

  1. distillationhad been freshly distilled over sodium hydroxide pellets
  2. temperatureThe mixture was then refluxed for a total of 12 hours
  3. customafter which the solvent (n-propanol) and excess hydrozine were removed at reduced pressure
  4. customThe residual crude hydrazone was recrystallized from ethanol

出典と根拠

ORDレコード
ord-0530283856734ca2b5ba798e6b0166fe
出典データセット
uspto-grants-1981_07
特許番号
US04280819

反応ノート

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