反応式
[CH2:1]([N:5]1[C:12](=[O:13])[CH:11]2[C:14]([CH3:16])([CH3:15])[CH:7]([C:8](=[O:18])[NH:9][C:10]2=[O:17])[C:6]1=[O:19])[CH2:2][CH2:3][CH3:4].C(=O)([O-])[O-].[K+].[K+].[CH3:26][C:27]1[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][C:28]=1[CH2:29]Cl>CN(C)C=O>[CH2:1]([N:5]1[C:6](=[O:19])[CH:7]2[C:14]([CH3:15])([CH3:16])[CH:11]([C:10](=[O:17])[N:9]([CH2:29][C:28]3[CH:31]=[C:32]([CH3:35])[CH:33]=[CH:34][C:27]=3[CH3:26])[C:8]2=[O:18])[C:12]1=[O:13])[CH2:2][CH2:3][CH3:4]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 120 °C
実験手順
2.6 g of 3-butyl-9,9-dimethyl-2,4,6, 8-tetraoxo-3,7-diazabicyclo[3,3,1]nonane were heated to 120° C. in 50 ml of dimethyl formamide with 1.7 g potassium carbonate for one hour. After cooling, a solution of 1.8 g of 2,5-dimethylbenzyl chloride in 20 ml of dimethyl formamide was added dropwise to the reaction mixture, and the reaction mixture was heated to 120° C. for another 3 hours. The reaction mixture was worked up by distilling off the dimethyl formamide, taking up the residue in dichloromethane, and washing with water adjusted to an alkaline pH value. The dichloromethane phase was separated, dried over magnesium sulfate, and concentrated. After recrystallizing the remaining crude product residue from ether/acetone, 1.2 g of 3-butyl-7-(2,5-dimethylbenzyl)-9, 9-dimethyl-2,4,6,8-tetraoxo-3,7diazabicyclo[3,3, 1]nonane was obtained having a melting point of 159-161° C.
後処理
- temperatureAfter cooling
- distillationby distilling off the dimethyl formamide
- washwashing with water
- customThe dichloromethane phase was separated
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customAfter recrystallizing the remaining crude product residue from ether/acetone
出典と根拠
- ORDレコード
- ord-bccb56bf66324b898297c0bd947294be
- 出典データセット
- uspto-grants-1992_11
- 特許番号
- US05164401
関連ノート
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