4-Chlorobenzoyl chloride → 4-Cyano-1-methyl-5-(p-chlorobenzoylthioureido)-pyrazole

HRID 375703ノート

反応式

HRID 375703 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[N-:11]=[C:12]=[S:13].[NH4+].[NH2:15][C:16]1[N:20]([CH3:21])[N:19]=[CH:18][C:17]=1[C:22]#[N:23]>CC(C)=O.O>[C:22]([C:17]1[CH:18]=[N:19][N:20]([CH3:21])[C:16]=1[NH:15][C:12]([NH:11][C:6](=[O:7])[C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][CH:4]=1)=[S:13])#[N:23]

参加物

6

反応物 3

HCID 85014-Chlorobenzoyl chlorideHCID 2197405-Amino-1-methyl-1H-pyrazole-4-carbonitrileHCID 178514171HCID 178514171、化合物

生成物 1

HCID 867492264-Cyano-1-methyl-5-(p-chlorobenzoylthioureido)-pyrazole収率 65%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

6.4 ml (50 mmol) of p-chlorobenzoyl chloride were added to a solution of 4.2 g (55 mmol) of ammonium isothiocyanate in 100 ml of acetone at about 20° C. Stirring was carried out for 30 minutes, after which a solution of 6.1 g (50 mmol) of 5-amino-4-cyano-1-methylpyrazole in 100 ml of acetone was slowly added dropwise at 50° C. This mixture was heated at the boil for 4 hours, cooled to about 25° C. and then diluted with 1000 ml of water. The product was extracted with ethyl acetate. Yield: 65%.

後処理

  1. temperatureThis mixture was heated at the boil for 4 hours
  2. extractionThe product was extracted with ethyl acetate

出典と根拠

ORDレコード
ord-1070cd6c4d1d44779b1534cb24d15279
出典データセット
uspto-grants-1996_01
特許番号
US05486618

反応ノート

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