Water → 5-Amino-3-ethyl-1-(2,4,6-trichlorophenyl)pyrazole-4-carboxamide

HRID 1860543

反応式

HRID 1860543 の反応式
[C:1]([C:3](=[C:7](OCC)[CH2:8][CH3:9])[C:4]([NH2:6])=[O:5])#[N:2].[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[C:15]=1[NH:22][NH2:23].O>CO>[NH2:2][C:1]1[N:22]([C:15]2[C:14]([Cl:13])=[CH:19][C:18]([Cl:20])=[CH:17][C:16]=2[Cl:21])[N:23]=[C:7]([CH2:8][CH3:9])[C:3]=1[C:4]([NH2:6])=[O:5]

参加物

5

反応物 3

HCID 962WaterHCID 79234(2,4,6-Trichlorophenyl)hydrazineHCID 545251922-Cyano-3-ethoxypentenamide

生成物 1

HCID 112560865-Amino-3-ethyl-1-(2,4,6-trichlorophenyl)pyrazole-4-carboxamide収率 82%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Part A: To a stirred solution of 320 mg (1.9 mmol) of 2-cyano-3-ethoxypentenamide in 7 mL of MeOH was added 465 mg (2.2 mmol) of 2,4,6-trichlorophenylhydrazine. The solution was stirred 3 h at reflux, treated with 2 mL of water, and allowed to stir an additional 1 h, cooling to RT. The white solid which precipitated was filtered, washed with 2:1 MeOH-water, and air-dried to afford 520 mg (82%) of 5-amino-3-ethyl-1-(2,4,6-trichlorophenyl)pyrazole-4-carboxamide, mp 186-188° C., Mass Spec (CI+): 331.9989 (M)+.

後処理

  1. temperatureat reflux
  2. stirringto stir an additional 1 h
  3. customThe white solid which precipitated
  4. filtrationwas filtered
  5. washwashed with 2:1 MeOH-water
  6. customair-dried

出典と根拠

ORDレコード
ord-672ff26dcf7b46a2a7d876ed2d45beb2
出典データセット
uspto-grants-2003_03
特許番号
US06531477B1

関連ノート

読み込み中…