Ammonia → HCID 178481735, 화합물

HRID 2182813

반응식

HRID 2182813 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])[NH:11][N:10]=1.S(OC)(O[CH3:19])(=O)=O.C(=O)([O-])[O-].[K+].[K+].N.Cl>C1(C)C=CC=CC=1>[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]([CH3:19])[N:10]=1

참가 물질

7

반응물 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 178515597HCID 178515597, 화합물

생성물 1

HCID 178481735HCID 178481735, 화합물수율 67.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

30 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole from Example 3.1 were initially charged in 750 ml of toluene. 23.1 g of dimethyl sulfate and 7.5 g of potassium carbonate were added, and the mixture was heated at reflux for 2 h. After cooling to room temperature, the mixture was made alkaline using ammonia and stirred overnight. The mixture was acidified by addition of hydrochloric acid (pH about 1) and cooled to room temperature, and the precipitated solid was filtered off. Drying gave 21.4 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1-methyl-1H-pyrazole (purity according to GC 99.2%, yield 66.8%). M.p.: 128° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 h
  3. temperaturecooled to room temperature
  4. filtrationthe precipitated solid was filtered off
  5. customDrying

출처 및 근거

ORD 기록
ord-7699cd7ee4c345c598cec46a2ba68854
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897322B2

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