Hydrochloric Acid → 4-(methoxycarbonyl)-2-methylthiophen-3-aminium chloride
反応式
[C:1]([CH:5]1[CH2:9][S:8][CH:7]([CH3:10])[C:6]1=[N:11]O)([O:3][CH3:4])=[O:2].[ClH:13]>CCOCC>[ClH:13].[NH2:11][C:6]1[C:5]([C:1]([O:3][CH3:4])=[O:2])=[CH:9][S:8][C:7]=1[CH3:10]参加物
4
実験手順
A solution of 41.1 g. (0.217 mole) of 4-carbomethoxy-3-keto-2-methyltetrahydrothiophene oxime in 600 ml. anhydrous ether, previously saturated with gaseous hydrogen chloride at 0°, was allowed to stir at 25° overnight. The separated solid was collected, washed well with ether, and dried to afford 33.2 g. Evaporation of the filtrate yielded after recrystallization of the residue an additional 4.2 g. to afford a total yield of pure 3-amino-4-carbomethoxy-2-methylthiophene hydrochloride of 37.4 g. (84%). The compound melts 191°-192°.
後処理
- customat 0°
- customThe separated solid was collected
- washwashed well with ether
- customdried
- customto afford 33.2 g
- customEvaporation of the filtrate
- customyielded
- customafter recrystallization of the residue an additional 4.2 g
出典と根拠
- ORDレコード
- ord-b11d41955b4040d9bff8fd8f6ffb7011
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04428963
反応ノート
読み込み中…