Pyridine → HCID 58724547、化合物

HRID 1393044ノート

反応式

HRID 1393044 の反応式
[CH3:1][N:2]1[C:6]([N:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)=[C:5]([C:12]([OH:14])=O)[CH:4]=[N:3]1.N1C=CC=CC=1.N1C(F)=NC(F)=NC=1[F:23]>ClCCl>[CH3:1][N:2]1[C:6]([N:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)=[C:5]([C:12]([F:23])=[O:14])[CH:4]=[N:3]1

参加物

5

反応物 3

HCID 1049PyridineHCID 12664Cyanuric fluorideHCID 155002461-Methyl-5-(1H-pyrrol-1-yl)-1H-pyrazole-4-carboxylic acid

生成物 1

HCID 58724547HCID 58724547、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred solution of 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid (7.65 g, 40 mmol) in dry dichloromethane (150 mL) and pyridine (3.2 mL, 40 mmol) under a nitrogen atmosphere was added cyanuric fluoride (5.4 g, 40 mmol) at 0° C. The reaction mixture was stirred for two hours during which time the reaction temperature was allowed to rise to room temperature. Crushed ice was then added along with additional dichloromethane. The organic layer was separated and the aqueous layer was extracted twice with dichloromethane. Concentration of the combined organic layers under reduced pressure gave 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carbonyl fluoride which was used in the next step without further purification.

後処理

  1. customto rise to room temperature
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted twice with dichloromethane

出典と根拠

ORDレコード
ord-dde0e4045b7648f1953776d2217ab9d5
出典データセット
uspto-grants-2008_03
特許番号
US07345058B2

反応ノート

読み込み中…