Nitric Acid → 5-Bromo-4,6-dimethyl-3-nitro-2-pyridinylamine
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1.[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[NH2:1][C:2]1[C:7]([N+:11]([O-:13])=[O:12])=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1参加物
4
実験手順
4 g (20 mmol) of the product obtained in Stage A are dissolved in 16 ml of concentrated sulfuric acid with stirring and cooling in ice. The solution is brought to 55° C. and 1.3 ml of concentrated nitric acid are added dropwise, care being taken to maintain the temperature between 55° and 60° C. The stirring is continued for 20 minutes and the mixture is then poured onto crushed ice. The product is precipitated by addition of 40% sodium hydroxide. It is filtered off, washed with water and then dried. 3.7 g of product are thus collected. The product is recrystallized from 95° C. ethanol.
後処理
- temperaturecooling in ice
- customis brought to 55° C.
- temperatureto maintain the temperature between 55° and 60° C
- additionthe mixture is then poured
- customonto crushed ice
- customThe product is precipitated by addition of 40% sodium hydroxide
- filtrationIt is filtered off
- washwashed with water
- customdried
- custom3.7 g of product are thus collected
- customThe product is recrystallized from 95° C. ethanol
出典と根拠
- ORDレコード
- ord-c6268f0f22a04bdc8c602ddee7371ca8
- 出典データセット
- uspto-grants-1998_01
- 特許番号
- US05712294
反応ノート
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