反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH:15]=[CH:14][C:13](=[O:16])[NH:12][C:11]2=[O:17])=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH-].[K+].Br[CH2:21][CH3:22]>CN(C)C(=O)C>[CH2:21]([N:12]1[C:13](=[O:16])[CH:14]=[CH:15][N:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[C:11]1=[O:17])[CH3:22]参加物
5
実験手順
A mixture of 3 parts of 1-(4-nitrophenyl)-2,4(1H,3H)-pyrimidinedione, 1,4 parts of potassium hydroxide and 67.5 parts of N,N-dimethylacetamide was stirred for 1 hour at room temperature under nitrogen atmosphere. 1.52 Parts of bromoethane were added and stirring was continued overnight at room temperature. The reaction mixture was poured into 100 parts of ice water. The product was filtered off and stirred in methanol. The product was filtered off and dried in vacuo at 60° C., yielding 2.4 parts (65.6%) of 3-ethyl-1-(4-nitro-phenyl)-2,4(1H,3H)-pyrimidinedione; mp. 182.5° C. (int. 24).
後処理
- stirringstirring
- waitwas continued overnight at room temperature
- filtrationThe product was filtered off
- stirringstirred in methanol
- filtrationThe product was filtered off
- customdried in vacuo at 60° C.
出典と根拠
- ORDレコード
- ord-d072a9a384e947f2a9bfee02dda21a87
- 出典データセット
- uspto-grants-1990_06
- 特許番号
- US04931444
関連ノート
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