Hydrochloric Acid → HCID 178427293, 화합물

HRID 1725118

반응식

HRID 1725118 반응식
[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

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 2723791Sodium p-toluenesulfinateHCID 178481735HCID 178481735, 화합물

생성물 1

HCID 178427293HCID 178427293, 화합물수율 90.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-68e6cd9d584143c7b9540d5fca4b52d2
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07488831B2

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