Hydrazine → N-(5-Amino-1,2,4-triazol-3-yl)-2-nitrobenzenesulfonamide

HRID 622825노트

반응식

HRID 622825 반응식
[C:1]([N:3]=[C:4](SC)[NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])#[N:2].[NH2:20][NH2:21]>C(#N)C>[NH2:2][C:1]1[NH:21][N:20]=[C:4]([NH:5][S:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])[N:3]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 178503935methyl N-cyano-N'-(2-nitrophenyl)sulfonylcarbamimidothioate

생성물 1

HCID 13772880N-(5-Amino-1,2,4-triazol-3-yl)-2-nitrobenzenesulfonamide수율 82.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 29.4 g (98.0 mmol) of N'-Cyano-N-(2-nitrophenylsulfonyl)-S-methylisothiourea in 100 ml of acetonitrile was treated with 6.2 ml (6.3 g, 0.20 mol) of anhydrous hydrazine. A mild exothermic reaction occurred as the reaction mixture became homogeneous. After stirring for 9 days the precipitated solid was collected by filtration and dried to afford 22.9 g of yellow solid. The crude product was recrystallized from HOAc to yield a total of 15.9 g (57 percent) of the desired product as a pale yellow solid, mp 255°-256° C. IR and 1H NMR spectra were consistent with the assigned structure.

후처리

  1. customA mild exothermic reaction
  2. filtrationwas collected by filtration
  3. customdried

출처 및 근거

ORD 기록
ord-f06807d1a19a44ada9fad2451cdbeb55
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772720

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