Hydrochloric Acid → HCID 178481944、化合物
反応式
[CH3:1][NH:2][C:3]([C:10]([F:13])([F:12])[F:11])=[CH:4][C:5](OCC)=[O:6].C[NH:15]N.Cl>O>[CH3:1][N:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[CH:4][C:5]([OH:6])=[N:15]1参加物
5
実験手順
A 50 ml. flask equipped with mechanical stirrer and reflux condenser was charged with 19.7 g of ethyl 3-methylamino-4,4,4-trifluoro-2-butenoate and 4.8 g of methylhydrazine and heated to 50°-65° C. for 2.75 hr., then to 40°-45° C. for 2 hr., and then allowed to cool to room temperature and stand overnight. The clear reaction mixture was taken up in 15 ml. of water and conc. hydrochloric acid added dropwise to pH 6.0-6.5 which required 5.2 ml. of acid. The precipitated product was collected by filtration and dried to obtain 7.06 g (42.5%) of product m.p. 127°-128.5° C.
後処理
- customflask equipped with mechanical stirrer
- temperaturereflux condenser
- temperatureheated to 50°-65° C. for 2.75 hr
- waitstand overnight
- filtrationThe precipitated product was collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-d5adaaa05297444daaf31e3fd61804e0
- 出典データセット
- uspto-grants-1990_10
- 特許番号
- US04964895
反応ノート
読み込み中…