反応式
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([N:8]=[C:9]([O:16]C)[C:10]([O:14]C)=[N:11]2)=[C:6]([CH2:18][N:19]([CH2:28][CH3:29])[CH:20]([P:22](=[O:27])([O:25]C)[O:23]C)[CH3:21])[CH:5]=1)([O-:3])=[O:2].C([Si](CC)(CC)[Br:33])C>ClCCl>[BrH:33].[O:14]=[C:10]1[C:9](=[O:16])[NH:8][C:7]2[C:12](=[CH:13][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=2[CH2:18][N:19]([CH2:28][CH3:29])[CH:20]([P:22](=[O:23])([OH:25])[OH:27])[CH3:21])[NH:11]1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
160 mg (0.37 mmol) of dimethyl N-(7-nitro-2,3-dimethoxyquinoxalin-5-ylmethyl)-α-(ethylamino)ethylphosphonate are dissolved in 8 ml of dichloromethane and stirred at room temperature for one hour with 0.19 ml (4 eq.) of triethylbromosilane. The solvent and excess reagent are evaporated and the residue is briefly dried in a high vacuum, dissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid, and stirred at room temperature for 18 hours. The reaction mixture is diluted with diethyl ether, and the solid is filtered off, washed with diethyl ether and dried. The title compound is obtained as a beige solid; m.p.=191° (dec.).
後処理
- customThe solvent and excess reagent are evaporated
- customthe residue is briefly dried in a high vacuum
- dissolutiondissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid
- additionThe reaction mixture is diluted with diethyl ether
- filtrationthe solid is filtered off
- washwashed with diethyl ether
- customdried
出典と根拠
- ORDレコード
- ord-805450e2d57f40898fcf73124a490141
- 出典データセット
- uspto-grants-2000_09
- 特許番号
- US06117873
関連ノート
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