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 was initially charged in 1,2-ethanediol (380 ml), and hydrazine hydrate (119.6 ml, 2.459 mol) was then added. The mixture was heated under reflux while stirring for 4 h. The product precipitated out in the course of cooling. Water (380 ml) was added to the yellow crystals, and extraction was effected by stirring at RT for 10 min. The suspension was then filtered with suction through a frit and washed through with water (200 ml) and with THF at −10° C. (200 ml). The residue was dried under high vacuum over phosphorus pentoxide.
後処理
- temperatureThe mixture was heated
- temperatureunder reflux
- customThe product precipitated out in the course
- temperatureof cooling
- additionWater (380 ml) was added to the yellow crystals, and extraction
- stirringby stirring at RT for 10 min
- filtrationThe suspension was then filtered with suction through a frit
- washwashed through with water (200 ml) and with THF at −10° C. (200 ml)
- dry with materialThe residue was dried under high vacuum over phosphorus pentoxide
出典と根拠
- ORDレコード
- ord-95c48b4bbeba4e2bb24d034a4279465a
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096592B2
反応ノート
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