Acetic Acid → 6-Chloro-2,3-dihydro-3-hydroxy-2-imino-4-pyrimidinamine
反応式
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH2:9])[N:3]=1.C(O)(=[O:12])C.OO>O1CCCC1>[NH2:9][C:4]1[N:3]([OH:12])[C:2](=[NH:1])[N:7]=[C:6]([Cl:8])[CH:5]=1参加物
5
実験手順
1.5 g (10 mmoles) of 2,6-diamino-4-chloropyrimidine are dissolved in 20 ml of anhydrous tetrahydrofuran. A mixture of 10 ml of acetic acid and 2 ml of a 70% aqueous hydrogen peroxide solution is added in 30 minutes under stirring and reflux. The reaction mixture is boiled for four hours, evaporated in vacuo to third of its volume, and a 40% aqueous sodium hydroxide solution is added to the residue until reaching a pH value of 8. The mixture is allowed to stand in refrigerator for a night. The crystals are filtered, washed with water and dried. In this way 1.0 g (63%) of the aimed compound is obtained.
後処理
- additionis added in 30 minutes
- temperaturereflux
- customevaporated in vacuo to third of its volume
- additiona 40% aqueous sodium hydroxide solution is added to the residue
- waitto stand in refrigerator for a night
- filtrationThe crystals are filtered
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-81cf548a2dde46caa3c84c40e1ce9f9a
- 出典データセット
- uspto-grants-1988_10
- 特許番号
- US04780537
反応ノート
読み込み中…