Acetic Acid → 4,6-Diaminopyrimidine-2-sulfinic acid
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]=[C:4]([SH:9])[N:3]=1.OO.C(O)(=[O:14])C.[OH-:16].[Na+]>>[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]=[C:4]([S:9]([OH:14])=[O:16])[N:3]=1参加物
5
実験手順
To a solution of 50 g of 4,6-diamino-2-mercaptopyrimidine (Aldrich, Milwaukee, Wis., USA) in 2N NaOH (220 mL) was added 750 mL of a 3% hydrogen peroxide solution. The solution was maintained at a temperature less than 20° C. Stirring was continued for a further 30 minutes and the clear pale yellow solution was acidified with acetic acid (ca. 50 mL). The precipitate was washed with H2O and air dried, to give 33 as 58 g (95 % yield) of an off-white amorphous acid (m.p. 168°-170° C. decomp.). For analysis, a sample was dissolved in dilute aqueous ammonia and reprecipitated with acetic acid.
後処理
- temperatureThe solution was maintained at a temperature less than 20° C
- washThe precipitate was washed with H2O and air
- customdried
出典と根拠
- ORDレコード
- ord-de605518dcb64f55a346b190ae6d938d
- 出典データセット
- uspto-grants-1997_03
- 特許番号
- US05612468
反応ノート
読み込み中…