一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 1-NAPHTHHYDRAZIDE
43038-45-5

1-NAPHTHHYDRAZIDE synthesis

5synthesis methods
1-NAPHTHOIC ACID METHYL ESTER

2459-24-7

1-NAPHTHHYDRAZIDE

43038-45-5

General procedure for the synthesis of 1-naphthylhydrazine from methyl 1-naphthalenecarboxylate: Methyl 1-naphthalenecarboxylate (0.52 g, 2.8 mmol) was dissolved in 15 mL of 98% hydrazine hydrate, fitted with an air condenser tube, and the reaction was stirred for 8 h at 110 °C. The reaction was carried out in the presence of an air condenser tube. Upon completion of the reaction, the mixture was cooled to room temperature and the precipitated crystalline solid was collected by filtration. The resulting solid was dissolved in ethyl acetate (EtOAc), and the organic phase was washed sequentially with water, saturated sodium bicarbonate (NaHCO3) solution and brine, and then concentrated under reduced pressure to remove the solvent. The product was purified by column chromatography (elution gradient: hexane/ethyl acetate 1:1; hexane/ethyl acetate 1:2) to give 0.38 g (73% yield) of white crystalline solid. Thin layer chromatography (TLC) Rf = 0.53 (unfolding agent: chloroform/methanol 10:1). Melting point 166-169 °C (literature value 166 °C).IR (KBr, cm-1): νmax 3280 (N-H), 1658 (C=O), 1606, 1588, 1524, 1261, 955.1H NMR (300 MHz, DMSO-d6): δ 9.69 (s, 1H, NH), 8.35-8.10 (m. 1H, Ar-H), 8.05-7.88 (m, 2H, Ar-H), 7.63-7.26 (m, 4H, Ar-H), 4.60 (s, 2H, NH2).13C NMR (75 MHz, DMSO-d6): δ 168.2 (C=O), 133.6, 133.3, 130.2, 130.1, 128.4, 128.4 126.8, 126.4, 125.6, 125.6, 125.2 (Ar-C).

-

Yield:-

Steps:

Multi-step reaction with 2 steps
1: benzyltriphenylphosphonium chloride; bis(tri-t-butylphosphine)palladium(0) / toluene / 24 h / 110 °C / 15201 Torr / Autoclave; Glovebox
2: hydrazine hydrate / toluene / 0 °C / Glovebox; Inert atmosphere

References:

Quesnel, Jeffrey S.;Kayser, Laure V.;Fabrikant, Alexander;Arndtsen, Bruce A. [Chemistry - A European Journal,2015,vol. 21,# 26,p. 9550 - 9555]

1-NAPHTHHYDRAZIDE Related Search:

商洛市| 东丰县| 民勤县| 册亨县| 永嘉县| 黑山县| 鱼台县| 安阳县| 沙坪坝区| 雅安市| 正宁县| 塘沽区| 津市市| 牟定县| 阳朔县| 临武县| 涞源县| 凉山| 汤原县| 香港 | 黑河市| 塔城市| 保德县| 新宁县| 蓝田县| 山阳县| 西乌珠穆沁旗| 东方市| 大化| 玉山县| 靖安县| 揭阳市| 蚌埠市| 镇远县| 马关县| 乡城县| 肇州县| 册亨县| 阳山县| 金乡县| 灵寿县|