関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 2-(Methyleneamino)acetonitrile | HCID 8015 | — |
| 反応物 | 2-Methyl-2-heptanol | HCID 12242 | — |
| 生成物 | 2-Amino-N-(1,1-dimethylhexyl)acetamide hydrogen fumarate | HCID 23454130 | — |
反応手順
To a solution of 2-methylheptan-2-ol (6.50 g.; 0.05 mole) in trifluoroacetic acid (20 ml) at -5° C. was added powdered methyleneaminoacetonitrile (3.40 g.; 0.05 mole) over 10 minutes. The slurry was allowed to warm to 10° C. and stirred until homogeneous (2 hours). After an additional 2 hours at 10° C., the reaction mixture was poured into water (100 ml) and the neutral material extracted with ether. The acid solution was basified with ammonia (pH 9-10) and the liberated base extracted into ether (3×80 ml). The combined extractswere dried over Na2SO4, filtered, and evaporated to dryness to give a colourless oil which was converted to the hydrogen fumarate salt, m.p. 156°-158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04277498 |
|---|
| 出典データセット | uspto-grants-1981_07 |
|---|
| ORD ID | ord-fbb3ebd3ca53498a90b9dace0ad8ae6c |
|---|
| 出典メモ | uspto-grants-1981_07 |
|---|