Diazomethane → 1-(4-Aminophenyl)-3-methyl-3-azabicyclo[3.1.0]hexane-2,4-dione

HRID 1904796ノート

反応式

HRID 1904796 の反応式
[N+:1](=[CH2:3])=[N-].[NH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]23[CH2:16][CH:15]2[C:14](=[O:17])N[C:12]3=[O:18])=[CH:7][CH:6]=1>CO>[NH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]23[CH2:16][CH:15]2[C:14](=[O:17])[N:1]([CH3:3])[C:12]3=[O:18])=[CH:9][CH:10]=1

参加物

4

反応物 2

HCID 9550DiazomethaneHCID 140689341-(4-Aminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

生成物 1

HCID 101713541-(4-Aminophenyl)-3-methyl-3-azabicyclo[3.1.0]hexane-2,4-dione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

An approx. 0.3 molar solution of diazomethane is added dropwise at 0° C. to a solution of 202 mg of 1-(4-aminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione in 10 ml of methanol. The reaction mixture is allowed to stand for 16 hours, concentrated, and partitioned twice between ethyl acetate and water. The organic phases are dried over magnesium sulfate, filtered and concentrated. The residue is crystallised from ethyl acetate/petroleum ether, affording the title compound which is identical with the title compound of Example 3(a).

後処理

  1. concentrationconcentrated
  2. custompartitioned twice between ethyl acetate and water
  3. dry with materialThe organic phases are dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue is crystallised from ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-2dc5d8f9ce894ff3b234158bdef31a88
出典データセット
uspto-grants-1989_06
特許番号
US04839379

反応ノート

読み込み中…