Acetylacetone → N-(5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidin-2-yl)-2-nitrobenzenesulfonamide

HRID 620661노트

반응식

HRID 620661 반응식
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([NH:7][S:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[N+:17]([O-:19])=[O:18])(=[O:10])=[O:9])[N:3]=1.[CH3:20][C:21](=O)[CH2:22][C:23](=O)[CH3:24]>C(O)(=O)C>[CH3:20][C:21]1[CH:22]=[C:23]([CH3:24])[N:6]2[N:5]=[C:4]([NH:7][S:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N+:17]([O-:19])=[O:18])(=[O:10])=[O:9])[N:3]=[C:2]2[N:1]=1

참가 물질

4

반응물 2

HCID 31261AcetylacetoneHCID 13772880N-(5-Amino-1,2,4-triazol-3-yl)-2-nitrobenzenesulfonamide

생성물 1

HCID 13772892N-(5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidin-2-yl)-2-nitrobenzenesulfonamide수율 82.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 2.43 g (9.00 mmol) of N-(5-amino-1,2,4-triazol-3-yl)-2-nitrobenzenesulfonamide and 1.85 ml (1.80 g, 18.0 mmol) of 2,4 pentanedione in 25 ml of glacial acetic acid was heated at reflux for 19 hours. After cooling to room temperature, the solid which separated was collected by filtration, washed with acetic acid and dried in vacuo to yield 2.58 g (82 percent) of the desired product as an off-white crystalline solid, mp 255°-256° C. IR and 1H NMR spectra were in agreement with the assigned structure.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 19 hours
  3. customthe solid which separated
  4. filtrationwas collected by filtration
  5. washwashed with acetic acid
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-39d4a2c859af46feb08887df9b8f5b0c
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822404

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