Ammonia → HCID 178481735、化合物

HRID 2182813

反応式

HRID 2182813 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])[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

参加物

7

反応物 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 178515597HCID 178515597、化合物

生成物 1

HCID 178481735HCID 178481735、化合物収率 67.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7699cd7ee4c345c598cec46a2ba68854
出典データセット
uspto-grants-2005_05
特許番号
US06897322B2

関連ノート

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