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Hydrazine → 4-(5-amino-1H-1,2,4-triazol-3-ylamino)-2,6-dichlorobenzonitrile

HRID 1486585
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인쇄 미리보기

반응식

HRID 1486585 반응식
[C:1](/[N:3]=[C:4](\SC)/[NH:5][C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([C:13]#[N:14])=[C:8]([Cl:15])[CH:7]=1)#[N:2].[NH2:18][NH2:19]>C(O)C>[NH2:2][C:1]1[NH:19][N:18]=[C:4]([NH:5][C:6]2[CH:11]=[C:10]([Cl:12])[C:9]([C:13]#[N:14])=[C:8]([Cl:15])[CH:7]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 178503893(Z)-methyl N'-cyano-N-(3,5-dichloro-4-cyanophenyl)carbamimidothioate

생성물 1

HCID 727067564-(5-amino-1H-1,2,4-triazol-3-ylamino)-2,6-dichlorobenzonitrile수율 71%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of (Z)-methyl N′-cyano-N-(3,5-dichloro-4-cyanophenyl)carbamimidothioate (234 mg, 821 μmol, Eq: 1.00) and hydrazine (263 mg, 258 μl, 8.21 mmol, Eq: 10) in ethanol (10 mL) was heated at 65° C. o/n. The reaction mixture was concentrated and chromatographed (23 Supelco, 100% DCM to 5% to 10% MeOH/DCM to give 156 mg (71%) of desired product as an off-white solid.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customchromatographed (23 Supelco, 100% DCM to 5% to 10% MeOH/DCM

출처 및 근거

ORD 기록
ord-db21468bb2414658aee4eaee8cc833e1
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428469B2

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