Water → 1-(4-aminosulphonylphenyl)-4,5-dihydro-5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole

HRID 1611858노트

반응식

HRID 1611858 반응식
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][NH2:12])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[F:13][C:14]([F:27])([F:26])[C:15](=O)/[CH:16]=[CH:17]/[C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=1.O>C(O)(=O)C>[NH2:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH:17]([C:18]3[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=3)[CH2:16][C:15]([C:14]([F:13])([F:26])[F:27])=[N:12]2)=[CH:9][CH:10]=1)(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 962WaterHCID 78105p-HydrazinobenzenesulphonamideHCID 11206657HCID 11206657, 화합물

생성물 1

HCID 99519571-(4-aminosulphonylphenyl)-4,5-dihydro-5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole수율 45%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 4-(aminosulphonyl)phenylhydrazine chlorohydrate (0.82 g, 3.69 mmoles) and (E)-1,1,1-trifluoro-4-(4-methylphenyl)-3-butene-2-one (0.79 g, 3.69 mmoles) in 15 ml of acetic acid is refluxed for 3 hours under a nitrogen atmosphere. It is cooled, poured over water and extracted with AcOEt. The organic solution is washed with water, dried over anhydrous sodium sulphatic and evaporated to dryness under vacuum. The crude product thus obtained is crystallised from EtOH-petrol ether to give 1-(4-aminosulphonylphenyl)-4,5-dihydro-5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole (0.65 g, yield: 45%).

후처리

  1. temperatureIt is cooled
  2. extractionextracted with AcOEt
  3. washThe organic solution is washed with water
  4. dry with materialdried over anhydrous sodium sulphatic
  5. customevaporated to dryness under vacuum
  6. customThe crude product thus obtained
  7. customis crystallised from EtOH-petrol ether

출처 및 근거

ORD 기록
ord-7bfdefa69557408e9c688f28031f52e3
출처 데이터셋
uspto-grants-2006_01
특허 번호
USRE038963E1

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