Acetic Anhydride → HCID 58371859, 화합물

반응식

Cl.[Br:2][C:3]1[CH:13]=[CH:12][C:6]([C:7](=[NH:11])[NH:8][NH:9][CH3:10])=[CH:5][CH:4]=1.C(O[C:18](=O)[CH3:19])(=O)C>>[Br:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]2[N:11]=[C:18]([CH3:19])[N:9]([CH3:10])[N:8]=2)=[CH:12][CH:13]=1

참가 물질

반응물 2

HCID 7918Acetic Anhydride

HCID 178486231HCID 178486231, 화합물

생성물 1

HCID 58371859HCID 58371859, 화합물

반응 조건

온도: 100 °C

실험 절차

A mixture of 4-bromo-N′-methylbenzimidohydrazide hydrochloride 1 (1.7 g) (prepared according to a procedure in synthesis of Sch-1499895) in acetic anhydride (10 ml) was heated at 100° C. for 0.5 hour. After cooling and concentration under reduced pressure, the residue was dissolved in EtOAc, washed with saturated NaHCO3 twice, brine and dried (MgSO4). After evaporation of solvent, the residue was purified on silica gel. Elution with EtOAc gave 3-(4-bromophenyl)-1,5-dimethyl-1H-[1,2,4]-triazole 2BK (1.04 g).

후처리

customprepared
temperatureAfter cooling
concentrationconcentration under reduced pressure
dissolutionthe residue was dissolved in EtOAc
washwashed with saturated NaHCO3 twice
dry with materialbrine and dried (MgSO4)
customAfter evaporation of solvent
customthe residue was purified on silica gel
washElution with EtOAc

출처 및 근거

ORD 기록: ord-656f3ea274ec4f639a79657aad1623b9
출처 데이터셋: uspto-grants-2014_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08716483B2

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