反応式
[CH:1]([NH:3][CH2:4][CH2:5][CH2:6][N:7]([CH3:14])[CH2:8][CH2:9][CH2:10][NH:11][CH:12]=[O:13])=[O:2].[CH3:15][O:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21][Cl:22])=[CH:19][C:18]=1[N+:25]([O-:27])=[O:26]>C(#N)C>[Cl-:22].[CH3:14][N+:7]([CH2:21][C:20]1[CH:23]=[CH:24][C:17]([O:16][CH3:15])=[C:18]([N+:25]([O-:27])=[O:26])[CH:19]=1)([CH2:6][CH2:5][CH2:4][NH:3][CH:1]=[O:2])[CH2:8][CH2:9][CH2:10][NH:11][CH:12]=[O:13]参加物
実験手順
A mixture of 54.0 parts of N,N-bis(3-formamidopropyl)methylamine, 50.4 parts of 4-methoxy-3-nitrobenzyl chloride, and 78 parts of acetonitrile was stirred at reflux for seven and a half hours. An additional 78 parts of acetonitrile was added to the reaction mixture causing an oil to separate. Heating at reflux was continued for an additional two hours and the 140 parts of acetonitrile was distilled away and 200 parts of water was added. The remaining acetonitrile was removed by distillation and the cooled reaction mixture was filtered with the aid of diatomaceous earth to obtain an aqueous solution of N-methyl-N-(3-nitro-4-methoxybenzyl)-N,N-bis(3-formamidopropyl)ammonium chloride. The solution was used directly for reduction of the nitro group.
後処理
- temperatureat reflux for seven and a half hours
- customto separate
- temperatureHeating
- temperatureat reflux
- distillationthe 140 parts of acetonitrile was distilled away
- addition200 parts of water was added
- customThe remaining acetonitrile was removed by distillation
- customthe cooled reaction mixture
- filtrationwas filtered with the aid of diatomaceous earth
出典と根拠
- ORDレコード
- ord-273833c9c1fc4afeb25732ae8da2b3d8
- 出典データセット
- uspto-grants-1977_12
- 特許番号
- US04065500
関連ノート
読み込み中…