Triethylamine → 1H-Pyrazole-4-carboxamide, 5-chloro-1-(3-chlorophenyl)-N-methyl-

HRID 1731262ノート

反応式

HRID 1731262 の反応式
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([OH:16])=O.[C:17](N1C=CN=C1)([N:19]1C=CN=C1)=O.Cl.CN.C(N(CC)CC)C>CN(C=O)C>[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([NH:19][CH3:17])=[O:16]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 6364545Methylamine hydrochlorideHCID 13821933HCID 13821933、化合物

生成物 1

HCID 1757891H-Pyrazole-4-carboxamide, 5-chloro-1-(3-chlorophenyl)-N-methyl-収率 51.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 5.7 g of 5-chloro-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylic acid and 5.4 g of carbonyldiimidazole in 150 ml DMF was stirred at room temperature for 20 minutes. Next, 3.0 g of methylamine hydrochloride and 4.4 g of triethylamine were added and the mixture was stirred at room temperature for 20 hours. The mixture was poured into ice water and the precipitated solid was collected by filtration and dried. The solid was recrystallized from toluene to provide 3.1 g of 5-chloro-1-(3-chlorophenyl)-N-methyl-1H-pyrazole-4-carboxamide. Yield 50%. mp=163°-165° C.

後処理

  1. filtrationthe precipitated solid was collected by filtration
  2. customdried
  3. customThe solid was recrystallized from toluene

出典と根拠

ORDレコード
ord-e00aaf0af2574905b4080e1f0c6ed877
出典データセット
uspto-grants-1986_11
特許番号
US04620865

反応ノート

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