Hydrazine hydrate (1:1) → 6-Hydrazinonicotinic acid

HRID 37445

反応式

HRID 37445 の反応式
Cl[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.O.[NH2:12][NH2:13]>O.Cl>[NH:12]([C:2]1[N:3]=[CH:4][C:5]([C:6]([OH:8])=[O:7])=[CH:9][CH:10]=1)[NH2:13]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 792226-Chloronicotinic acid

生成物 1

HCID 37826176-Hydrazinonicotinic acid収率 77%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

6-Chloronicotinic acid (8.0g) was added to 85% hydrazine hydrate (35 ml). The reaction mixture was placed in a 100° C. oil bath for 4 hours. The homogeneous reaction mixture was concentrated to dryness to give a white solid. The solid was dissolved in water and on acidification to pH 5.5 with concentrated hydrochloric acid a precipitate formed. The precipitate was isolated by filtration and the solid was washed with 95% ethanol and ether to give 6.0 g of a pale brown solid; yield 77% m.p. 292°-293° C.;

後処理

  1. customwas placed in a 100° C.
  2. customfor 4 hours
  3. concentrationThe homogeneous reaction mixture was concentrated to dryness
  4. customto give a white solid
  5. customformed
  6. customThe precipitate was isolated by filtration
  7. washthe solid was washed with 95% ethanol and ether

出典と根拠

ORDレコード
ord-1f104d5265844ae6880da6034be833ba
出典データセット
uspto-grants-1995_05
特許番号
US05420285

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