156939-62-7
156939-62-7 結(jié)構(gòu)式
基本信息
N-芴甲氧羰基甘氨醛
(9H-芴-9-基)甲基2-氧代乙基氨基甲酸酯
(9H-芴-9-基)METHYL 2-乙基氨基甲酸
N-9-Fluorenylmethoxycarbonylglycinaldehyde
(9H-Fluoren-9-yl)methyl 2-oxoethylcarbamate
9H-fluoren-9-ylmethyl N-(2-oxoethyl)carbamate
2-[[(9-Fluorenylmethoxy)carbonyl]amino]acetaldehyde
Carbamic acid, N-(2-oxoethyl)-, 9H-fluoren-9-ylmethyl ester
物理化學(xué)性質(zhì)
制備方法
105496-31-9
156939-62-7
以2-(N-芴甲氧羰基氨基)乙醇為原料合成N-芴甲氧羰基甘氨醛的一般步驟:向2-(N-芴甲氧羰基氨基)乙醇(5.0g,18mmol)的二氯甲烷(50mL)懸浮液中加入二異丙基乙胺(12.4mL,70.6mmol)。將反應(yīng)混合物冷卻至-40℃,并在15分鐘內(nèi)逐滴加入三氧化硫吡啶絡(luò)合物(11.2g,70.6mmol)的二甲基亞砜(49.5mL)溶液。在-40℃下持續(xù)攪拌1小時(shí)后,用冰水和飽和食鹽水的混合液淬滅反應(yīng)。減壓濃縮除去有機(jī)溶劑,過濾收集生成的灰白色沉淀,并在真空下干燥。最后,通過硅膠快速柱色譜法進(jìn)行純化,以乙酸乙酯/己烷(1:1,v/v)為洗脫劑,得到N-芴甲氧羰基甘氨醛(4.7g,收率94%)。
參考文獻(xiàn):
[1] Organic Letters, 2002, vol. 4, # 17, p. 3001 - 3003
[2] Synthetic Communications, 2007, vol. 37, # 20, p. 3493 - 3499
[3] Patent: WO2018/149419, 2018, A1. Location in patent: Paragraph 001283; 001284
[4] European Journal of Organic Chemistry, 2008, # 34, p. 5786 - 5797
[5] Patent: WO2006/66183, 2006, A2. Location in patent: Page/Page column 63
