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

HRID 1904793ノート

反応式

HRID 1904793 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-7b402f1f1e9547a4a06726842231205c
出典データセット
uspto-grants-1989_06
特許番号
US04839379

反応ノート

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