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 Benzoic acid, 2-hydroxy-4-nitro-, ethyl ester
78987-51-6

Benzoic acid, 2-hydroxy-4-nitro-, ethyl ester synthesis

4synthesis methods
-

Yield:78987-51-6 89%

Reaction Conditions:

with thionyl chloride at 0 - 20;Product distribution / selectivity;Heating / reflux;

Steps:

1.c; 2.c; 3.c; 4.d

c. Synthesis of intermediate E; To a solution of anhydrous ethanol (500 ml) was charged D (50 g, 0.27 mol) and the reaction mixture was cooled to 0-5 0C at which time thionyl chloride (59.6 ml, 0.81 mol) was slowly added to keep the reaction mixture temperature < 20 0C. After complete thionyl chloride addition the reaction mixture was heated to reflux and maintained at reflux overnight. The reaction mixture was cooled to 20 0C and then concentrated to an oil by evaporation under reduced pressure. To the residue was charged a mixture of water (200 ml) and ethyl acetate (200 ml). The layers were separated and the aqueous was extracted with additional ethyl acetate (2 x 200 ml). The combined organic layers were washed with 10% sodium bicarbonate solution (200 ml), water (200 ml) and brine (200 ml) and then dried over sodium sulfate, filtered and concentrated under reduced pressure to give E as a yellow solid (51 g, 89%).; c. Synthesis of Intermediate E; To a solution of anhydrous ethanol (250 ml) was charged intermediate D (25 g, 0.137 mol) and the reaction mixture was cooled to 0-5 C at which time thionyl chloride (29.8 ml, 0.41 mol) was slowly added to keep the reaction mixture temperature < 20 C. After complete thionyl chloride addition the reaction mixture was heated to reflux and maintained at reflux overnight. The reaction mixture was cooled to 20 C and then concentrated to an oil by evaporation under reduced pressure. To the residue was charged a mixture of water (100 ml) and ethyl acetate (100 ml). The layers were separated and the aqueous was extracted with additional ethyl acetate (2 x 100 ml). The combined organic layers were washed with 10% sodium bicarbonate solution (100 ml), water (100 ml) and brine (100 ml) and then dried over sodium sulfate, filtered and concentrated under reduced pressure to give intermediate E as a yellow solid (27 g, 93%).; c. Synthesis of intermediate E; To a solution of anhydrous ethanol (500 ml) was charged intermediate D (50 g, 0.27 mol) and the reaction mixture was cooled to 0-5 C at which time thionyl chloride (59.6 ml, 0.81 mol) was slowly added to keep the reaction mixture temperature < 20 C. After complete thionyl chloride addition the reaction mixture was heated to reflux and maintained at reflux overnight. The reaction mixture was cooled to 20 C and then concentrated to an oil by evaporation under reduced pressure. To the residue was charged a mixture of water (200 ml) and ethyl acetate (200 ml). The layers were separated and the aqueous was extracted with additional ethyl acetate (2 x 200 ml). The combined organic layers were washed with 10% sodium bicarbonate solution (200 ml), water (200 ml) and brine (200 ml) and then dried over sodium sulfate, filtered and concentrated under reduced pressure to give intermediate E as a yellow solid (51 g, 89%).; d. Synthesis of common intermediate G; To a solution of a protic polar solvent, such as ethanol, is charged 2-hydroxy- 4-nitrobenzoic acid followed by a chlorinating agent such as thionyl chloride. After reflux for 8-16 hours the reaction mixture is concentrated and extracted with an organic solvent such as ethyl acetate, washed with sodium carbonate solution, water and brine and the organic evaporated in vacuo to afford the product as a yellow solid.

References:

WO2008/11539,2008,A2 Location in patent:Page/Page column 36; 40; 44; 48

施甸县| 望都县| 神木县| 郧西县| 平山县| 揭阳市| 大足县| 信丰县| 建湖县| 蓝田县| 西和县| 海门市| 神农架林区| 湖口县| 左贡县| 城口县| 兴业县| 交城县| 阿勒泰市| 台中县| 信丰县| 阿拉善盟| 沙湾县| 东乡县| 安图县| 凤台县| 广州市| 文化| 乌兰察布市| 枣庄市| 洪湖市| 通渭县| 阜平县| 酉阳| 景谷| 平乡县| 沈阳市| 蒲江县| 绵竹市| 鲁山县| 怀仁县|