反応 #65723

ord-1f104d5265844ae6880da6034be833ba

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was placed in a 100° C.
  2. 2
    その他for 4 hours
  3. 3
    濃縮The homogeneous reaction mixture was concentrated to dryness
  4. 4
    その他to give a white solid
  5. 5
    その他formed
  6. 6
    その他The precipitate was isolated by filtration
  7. 7
    洗浄the solid was washed with 95% ethanol and ether

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.;

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05420285uspto-grants-1995_05