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Hydrazine hydrate (1:1) → N-(5-Amino-1,2,4-triazol-3-yl)-2,5-dichlorobenzenesulfonamide

HRID 620663
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HRID 620663 반응식
[C:1]([N:3]=[C:4](SC)[NH:5][S:6]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[Cl:16])(=[O:8])=[O:7])#[N:2].O.[NH2:20][NH2:21]>C(O)C>[NH2:2][C:1]1[NH:21][N:20]=[C:4]([NH:5][S:6]([C:9]2[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=2[Cl:16])(=[O:8])=[O:7])[N:3]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 178503936HCID 178503936, 화합물

생성물 1

HCID 13772881N-(5-Amino-1,2,4-triazol-3-yl)-2,5-dichlorobenzenesulfonamide수율 63.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 8.51 g (26.2 mmol) of N'-cyano-N-(2,5-dichlorophenylsulfonyl)-S-methylisothiourea and 10 ml (10 g, 0.20 mol) of hydrazine monohydrate in 85 ml of ethanol was heated at reflux for 30 minutes. After cooling to room temperature, the solid which separated was collected and suspended in 170 ml of H2O and the suspension was acidified with concentrated aqueous HCl. After stirring the suspension for 4 hours the solid was collected and dried in vacuo to yield 5.10 g (57 percent) of the desired product as a hydrochloride salt, mp 306°-308° C. IR and 1H NMR spectra were consistent with the assigned structure.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 30 minutes
  3. customthe solid which separated
  4. customwas collected
  5. customwas collected
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-1d0b89fa78464881b04fbfc852393bf5
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822404

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