Hydrazine hydrate (1:1) → HCID 178509230、化合物
反応式
Cl[C:2]1[N:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[C:4]#[N:5].O.[NH2:12][NH2:13]>C(O)CO>[F:10][C:7]1[CH:6]=[C:3]2[C:4]([NH2:5])=[N:13][NH:12][C:2]2=[N:9][CH:8]=1参加物
4
実験手順
A suspension of 38.5 g (245.93 mmol) of 2-chloro-5-fluoronicotinonitrile in 1,2-ethanediol (380 ml) was prepared and then hydrazine hydrate (119.6 ml) was added. It was heated under reflux for 4 h, with stirring. On cooling, the product was precipitated. Water (380 ml) was added to the crystals and it was left to precipitate for 10 min at RT. Then the suspension was filtered with suction on a frit, and washed again with water (200 ml) and with cold (−10° C.) THF (200 ml). Drying over phosphorus pentoxide under high vacuum.
後処理
- customwas prepared
- temperatureIt was heated
- temperatureunder reflux for 4 h
- temperatureOn cooling
- customthe product was precipitated
- additionWater (380 ml) was added to the crystals and it
- waitwas left
- customto precipitate for 10 min at RT
- filtrationThen the suspension was filtered with suction on a frit
- washwashed again with water (200 ml) and with cold (−10° C.) THF (200 ml)
- dry with materialDrying over phosphorus pentoxide under high vacuum
出典と根拠
- ORDレコード
- ord-abde68c3ca77470c9033206fa70d51ac
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859569B2
反応ノート
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