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

HRID 1904796노트

반응식

HRID 1904796 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2dc5d8f9ce894ff3b234158bdef31a88
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839379

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