4-Bromo-2,6-dinitroaniline → 5-Bromo-3-nitrobenzene-1,2-diamine

온도

90 °C

4-bromo-2,6-dinitrobenzenamine was dissolved in EtOH (50 mL) and (NH4)2S (2.2 mL) was added to the mixture. The reaction mixture was heated to 90° C. for 1 h. TLC showed a new compound and some remaining starting material remained. Additionally, another batch (NH4)2S (2.5 mL) was added. After 1 h, TLC analysis showed little starting material remained. The reaction mixture was concentrated to give a deep red solid. It was then purified by silica gel chromatography eluted with DCM to afford the desired product as a red solid (578 mg, 50%). 1H NMR (300 MHz, CDCl3) δ ppm 3.50 (br s, 2H), 5.93 (br s, 2H), 7.04 (d, 1H, J=1.8 Hz), 7.87 (d, 1H, J=1.8 Hz); LC-MS: m/e=232 [M+1]+.

1. concentrationThe reaction mixture was concentrated
2. customto give a deep red solid
3. customIt was then purified by silica gel chromatography
4. washeluted with DCM

ORD 기록

ord-445d06d6f59542d1babeea0e30cd1b06

출처 데이터셋

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08865912B2