Hydrazine → HCID 178465624、化合物

HRID 1378910ノート

反応式

HRID 1378910 の反応式
I.CS[C:4](=[NH:13])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[CH:7]=1.[NH2:14][NH2:15].[C:16]([C:19]1[N:27]=[CH:26][CH:25]=[CH:24][C:20]=1[C:21]([OH:23])=[O:22])(=O)[CH3:17]>C(O)C.CO>[CH3:17][C:16]([C:19]1[C:20]([C:21]([OH:23])=[O:22])=[CH:24][CH:25]=[CH:26][N:27]=1)=[N:14][NH:15][C:4](=[NH:13])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[CH:7]=1

参加物

6

反応物 3

HCID 9321HydrazineHCID 101762782-Acetyl-3-pyridinecarboxylic acidHCID 178503998HCID 178503998、化合物

生成物 1

HCID 178465624HCID 178465624、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

A mixture of the above isothiourea salt (8.5 g, 27.0 mmol) and hydrazine (1.4 g, 27.0 mmol) in 80 ml of ethanol is heated to reflux for 4 hr. The mixture is cooled and the solvent removed. The residue is diluted with 80 ml of water and filtered. A 20 ml aliquot of the resulting aqueous filtrate (2.0 g, 11.9 mmol) is mixed with 2-acetylnicotinic acid (2.0 g, 11.9 mmol) in 6 ml of methanol and stirred at RT overnight. A bright yellow solid is collected by filtration and dried to give 2-[methyl(3-carboxy-2-pyridyl)methylene]-N-(3-fluorophenyl)hydrazinecarboximidamide, (compound 16).

後処理

  1. temperatureis heated
  2. temperatureto reflux for 4 hr
  3. temperatureThe mixture is cooled
  4. customthe solvent removed
  5. additionThe residue is diluted with 80 ml of water
  6. filtrationfiltered
  7. filtrationA bright yellow solid is collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-fffb9758b7cb4c2ebf765f946918c9d6
出典データセット
uspto-grants-1997_09
特許番号
US05670456

反応ノート

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