Ethanol → 1-(4-Acetylaminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

HRID 1904793노트

반응식

HRID 1904793 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]23[CH2:20][CH:19]2[C:18](=[O:21])[NH:17][C:16]3=[O:22])=[CH:11][CH:10]=1.CN(CCC)C.C(O)C>O1CCCC1>[C:1]([NH:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]23[CH2:20][CH:19]2[C:18](=[O:21])[NH:17][C:16]3=[O:22])=[CH:13][CH:14]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 702EthanolHCID 7918Acetic AnhydrideHCID 61236N,N-DimethylpropylamineHCID 140689341-(4-Aminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

생성물 1

HCID 140689461-(4-Acetylaminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2.4 ml of acetic anhydride in 10 ml of tetrahydrofuran is added dropwise to a solution of 4 g of 1-(4-aminophenyl)-3-azabicyclo[3.1.0]hexane-2,4-dione and 120 mg of dimethylaminopropane in 150 ml of tetradrofuran, and the mixture is stirred overnight at room temperature. Then 0.5 ml of ethanol is added to the reaction mixture, which is stirred for 1 hour and filtered. The crystals so obtained are washed with tetrahydrofuran and ether, affording white crystals of the title compound with a melting point above 230° C. and Rf=0.3 in thin-layer silica gel plates in the system methylene chloride/methanol (10:1).

후처리

  1. stirringis stirred for 1 hour
  2. filtrationfiltered
  3. customThe crystals so obtained
  4. washare washed with tetrahydrofuran and ether

출처 및 근거

ORD 기록
ord-7b402f1f1e9547a4a06726842231205c
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839379

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