Water → HCID 178432418、化合物
反応式
Cl[C:2]1[N:9]=[C:8]([CH3:10])[C:7]([F:11])=[CH:6][C:3]=1[C:4]#[N:5].O.[NH2:13][NH2:14].C(N(C(C)C)CC)(C)C.O>C(O)CO.C(OCC)(=O)C>[F:11][C:7]1[CH:6]=[C:3]2[C:4]([NH2:5])=[N:14][NH:13][C:2]2=[N:9][C:8]=1[CH3:10]参加物
7
実験手順
58 g (340.027 mmol) of 2-chloro-5-fluoro-6-methylnicotinonitrile (preparation described in WO2007/41052, example U-2, page 80) was put in 1,2-ethanediol (580 ml) and then hydrazine hydrate (24.813 ml) and 56.091 ml (340.027 mmol) of diisopropyl ethylamine were added. The reaction mixture was heated with stirring for 16 h to 80° C. and then for 66 h to 120° C. After cooling, water (2.5 l) and ethyl acetate (2.5 l) were added and it was filtered with suction. The solid obtained was dried. 28.4 g (47% of theor.) of the target compound was obtained.
後処理
- temperatureThe reaction mixture was heated
- temperatureAfter cooling
- filtrationit was filtered with suction
- customThe solid obtained
- customwas dried
- custom28.4 g (47% of theor.) of the target compound was obtained
出典と根拠
- ORDレコード
- ord-46d380f521344b89b61d1c4d5f3ef297
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859569B2
反応ノート
読み込み中…