Potassium Iodide → HCID 19043019、化合物
反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[CH:4][CH:3]=1.[NH:10]1[CH:14]=[N:13][CH:12]=[N:11]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)=O>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][N:10]2[CH:14]=[N:13][CH:12]=[N:11]2)=[CH:4][CH:3]=1参加物
6
実験手順
A mixture of 1 g of 4-bromobenzyl bromide, 0.41 g of 1,2,4-triazole, 0.55 g of potassium carbonate and 33 mg of potassium iodide in 30 ml of acetone is stirred for 20 hours at 50°. The solid material is removed by filtration and the solution is concentrated by evaporation. The resulting crude precursor (1) is purified by column chromatography (SiO2, hexane/ethyl acetate 1:1) and crystallised from ether; m.p. 77°-79°; 1H-NMR (CDCl3): δ=5.3 (2H,s), 7.15 and 7.5 (4H,m), 7.95 (1H,s), 8.08 (1H,m).
後処理
- customThe solid material is removed by filtration
- concentrationthe solution is concentrated by evaporation
- customThe resulting crude precursor (1) is purified by column chromatography (SiO2, hexane/ethyl acetate 1:1)
- customcrystallised from ether
出典と根拠
- ORDレコード
- ord-99bbea2ccea5473a860bbf896237c520
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05583128
反応ノート
読み込み中…