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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1949840생성일: 2026년 10월 26일

Toluene → 3-(9-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-4-(2,4-difluorophenyl)-4H-1,2,4-triazole

https://huagongshe.com/reaction/1949840

반응식

참여 물질

역할이름HCID투입량
반응물TolueneHCID 1140—
반응물Dimethylformamide dimethyl acetalHCID 78373—
반응물2,4-Difluorophenylhydrazine hydrochlorideHCID 2733301—
반응물9-Bromo-4,5-dihydro-6-oxa-1-thia-benzo[e]azulene-2-carboxylic acid amideHCID 66868537—
용매Acetic AcidHCID 176—
용매WaterHCID 962—
용매DichloromethaneHCID 6344—
생성물3-(9-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-4-(2,4-difluorophenyl)-4H-1,2,4-triazoleHCID 57900350—

반응 조건

온도100 °C

반응 단계

A mixture of 9-bromo-4,5-dihydro-6-oxa-1-thia-benzo[e]azulene-2-carboxylic acid amide (340 mg), dimethylformamide dimethyl acetal (3 ml) and toluene (2.5 mL) was heated to 100° C. for 16 hours. The solvent was then reduced in vacuo and dissolved in acetic acid (3 ml) and water (0.3 mL) and to this was added 2,4-difluorophenylhydrazine hydrochloride (265 mg). The reaction mixture was heated to 100° C. for 3 hours. The reaction mixture was then cooled, and then diluted with dichloromethane, washed with sodium carbonate solution, dried (MgSO4) and the solvent removed in vacuo. Purification using flash chromatography yielded 293. NMR: (CDCl3): 3.15 (2H, t), 4.31 (2H, t), 6.82 (1H, d), 6.86 (1H, s), 7.08-7.13 (2H, m), one proton under chloroform peak, 7.72 (1H, s), 8.10 (1H, s)

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08399690B2
출처 데이터셋uspto-grants-2013_03
ORD IDord-d9e78001157f4f338faa0e06d2e450cb
출처 메모uspto-grants-2013_03