Hydrochloric Acid → HCID 178427293、化合物

HRID 1725118

反応式

HRID 1725118 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:13]=[C:12]([OH:14])[N:11]([CH3:15])[N:10]=1.[OH-].[Na+].[CH2:18]=O.[C:20]1([CH3:29])[CH:25]=[CH:24][C:23]([S:26]([O-:28])=[O:27])=[CH:22][CH:21]=1.[Na+].Cl>C(O)C.O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:13]([CH2:18][S:26]([C:23]2[CH:24]=[CH:25][C:20]([CH3:29])=[CH:21][CH:22]=2)(=[O:28])=[O:27])=[C:12]([OH:14])[N:11]([CH3:15])[N:10]=1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 2723791Sodium p-toluenesulfinateHCID 178481735HCID 178481735、化合物

生成物 1

HCID 178427293HCID 178427293、化合物収率 90.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

3-(2,4-Dichlorophenyl)-5-hydroxy-1-methylpyrazole (1.3 g (5 mmol)) synthesized in Reference Example 6 and 0.3 g (7.5 mmol) of sodium hydroxide were dissolved in 5 mL of ethanol. While stirring the resulting solution at room temperature, 1.0 g (11 mmol) of a 35% formalin solution was added dropwise thereto, followed by stirring at the same temperature for 1 hour. Subsequently, 0.9 g (5 mmol) of sodium p-toluenesulfinate was charged thereto at room temperature, and the obtained mixture was stirred for 2 hours. After the reaction, 2.5 g (25 mmol) of 35% hydrochloric acid was added dropwise thereto, 15 mL of water was further added, and the precipitated crystal was collected by filtration, washed twice with 10 mL of water and dried by a hot air drier to obtain 2.1 g (yield: 90.3%) of the title compound as a pale yellow crystal.

後処理

  1. stirringby stirring at the same temperature for 1 hour
  2. stirringat room temperature, and the obtained mixture was stirred for 2 hours
  3. additionwas added dropwise
  4. filtrationthe precipitated crystal was collected by filtration
  5. washwashed twice with 10 mL of water
  6. customdried by a hot air drier

出典と根拠

ORDレコード
ord-68e6cd9d584143c7b9540d5fca4b52d2
出典データセット
uspto-grants-2009_02
特許番号
US07488831B2

関連ノート

読み込み中…