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Benzoyl chloride → HCID 14155371, 화합물

HRID 619945
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HRID 619945 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]2[N:8]=[C:9]([S:11]([NH:14][C:15]3[C:20]([Cl:21])=[CH:19][CH:18]=[CH:17][C:16]=3[Cl:22])(=[O:13])=[O:12])[N:10]=[C:4]2[N:3]=1.C([O-])([O-])=O.[K+].[K+].[C:29](Cl)(=[O:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CC(C)=O>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]2[N:8]=[C:9]([S:11]([N:14]([C:29](=[O:36])[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[C:15]3[C:16]([Cl:22])=[CH:17][CH:18]=[CH:19][C:20]=3[Cl:21])(=[O:13])=[O:12])[N:10]=[C:4]2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7412Benzoyl chlorideHCID 11430Potassium CarbonateHCID 14155248HCID 14155248, 화합물

생성물 1

HCID 14155371HCID 14155371, 화합물수율 72%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A mixture of 3.00 g (8.37 mmol) of 5-methyl -N-(2,6-dichlorophenyl)-1,2,4-triazolo[1,5-a]pyrimidine-2-sulfonamide and 1.16 g (8.37 mmol) of anhydrous powdered K2CO3 in 100 ml of acetone was heated at reflux for 30 minutes. A solution of 1.18 g (8.37 mmol) of benzoyl chloride in 10 ml of acetone was added, and the reaction was heated at reflux for 115 min. The reaction was filtered, and the filtrate was evaporated at reduced pressure. The solid residue was collected by filtration, washed thoroughly with aqueous NaHCO3 and H2O and dried to yield 2.7, g (72%) of the desired product as a solid, mp 187°-189° C. IR and 1H NMR spectra were in agreement with the assigned structure.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 30 minutes
  3. temperaturethe reaction was heated
  4. temperatureat reflux for 115 min
  5. filtrationThe reaction was filtered
  6. customthe filtrate was evaporated at reduced pressure
  7. filtrationThe solid residue was collected by filtration
  8. washwashed thoroughly with aqueous NaHCO3 and H2O
  9. customdried
  10. customto yield 2.7

출처 및 근거

ORD 기록
ord-8e883acbe3094435a6ecc6ed980e335c
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04818273

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