897957-06-1

基本信息
6-溴-1-甲基二氫-2-酮
6-溴-1-甲基吲哚啉-2-酮
6-溴-1-甲基-2,3-二氫-1H-吲哚-2-酮
6-bromo-1-methyl-3H-indol-2-one
6-bromo-1-methyl-1,3-dihydro-indol-2-one
6-bromo-1-methyl-2,3-dihydro-1H-indol-2-one
6-bromo-1-methyl-1,3-dihydro-2H-indol-2-one
2H-Indol-2-one, 6-bromo-1,3-dihydro-1-methyl-
物理化學(xué)性質(zhì)
制備方法

667463-64-1

897957-06-1
以6-溴-1-甲基吲哚-2,3-二酮為原料合成6-溴-1-甲基二氫-2-酮的一般步驟:將6-溴-1-甲基吲哚-2,3-二酮(397 mg,1.65 mmol)與水合肼(1 mL,20.6 mmol)混合,加熱至100℃反應(yīng)1小時(shí),隨后升溫至125℃繼續(xù)反應(yīng)1小時(shí)。反應(yīng)完成后,將混合物冷卻至室溫,加入二氯甲烷(DCM)和水進(jìn)行分層。水層用DCM萃取兩次,合并有機(jī)層,用飽和食鹽水洗滌,無水硫酸鈉干燥。減壓濃縮有機(jī)相,所得殘余物通過柱色譜法純化,洗脫劑為環(huán)己烷/乙酸乙酯(3:1,v/v)。產(chǎn)物收率為65%。質(zhì)譜分析顯示:m/z 226 [M + H]+,m/z 224 [M + H]-,保留時(shí)間(rt)為0.58分鐘(LC-MS方法b)。
參考文獻(xiàn):
[1] Patent: WO2013/41497, 2013, A1. Location in patent: Page/Page column 36
[2] Patent: WO2014/140075, 2014, A1. Location in patent: Page/Page column 215; 217
[3] Patent: WO2014/140081, 2014, A1. Location in patent: Page/Page column 61; 62
[4] Patent: US2014/275159, 2014, A1. Location in patent: Paragraph 0328; 0331
[5] Patent: WO2014/140091, 2014, A1. Location in patent: Page/Page column 74; 75