関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Diamino-5-(4-amino-3,5-dimethoxy-benzyl)-6-chloropyrimidine | HCID 21280993 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 触媒 | Mercuric Chloride | HCID 24085 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Aditeren | HCID 176875 | — |
反応手順
A solution of 0.1 g. of mercury (II) chloride in 2 ml. of water and 1.5 g. of zinc powder was added to a solution of 1.5 g. of 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-6-chloropyrimidine in 15.5 ml. of glacial acetic acid and the mixture was boiled under reflux with stirring overnight. Then, the mixture was filtered while hot and the zinc powder washed with 5 ml. of acetic acid. The combined filtrates were added dropwise with stirring at a temperature below 20° C. to 40 ml. of concentrated ammonia. Then, the mixture was stirred at 20° C. for an additional hour and the solid material was removed by filtration under vacuum, washed with water, dried, recrystallized from methanol and there was obtained 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-pyrimidine having a melting point of 214° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04659818 |
|---|
| 出典データセット | uspto-grants-1987_04 |
|---|
| ORD ID | ord-bfe4c1946eee4587b120676a9c00f983 |
|---|
| 出典メモ | uspto-grants-1987_04 |
|---|